We’re reporting out on news from the 2020 AOAC INTERNATIONAL Virtual Annual Meeting in this live blog. See the Annual Meeting Schedule – and don’t forget to check this blog regularly to get the latest on new science at the Annual Meeting. Most recent updates will appear at the top of the page. All times are in U.S. Eastern Time.
Jump to updates:
September 24 – Testing for Life Student Symposium – Hot Topic Symposium COVID 19 – Concluding Remarks
September 23 – CBD/Hemp Testing – Food, Beverage, & Chemometrics – Food Allergen & Glutens – Salmonella Re-Emergence
September 22 – AOAC Spotlight – Probiotic Quality Standards – Innovative Technology and Data – Novel Cannabis and Botanicals Methods
September 21 – PFAS Methods – Dietary Supplements – Food Fraud – Vaping
September 18 – Ergot Alkaloids – PCR Quantification
Elemental Analysis as Markers for Food-Safety – Glyphosate Project Launch – Reference Materials in the AOAC Process – Novel Methods for Contaminants
Quality by Design – Tattoo Inks – High Resolution Mass Spectrometry – Probiotics
Natural Food Coloring – Mobile Botanical Identification – Quality Assurance of Quant PCR – Seafood Decomposition
Welcome, Keynote Address and Awards – Wiley Award Address – Wiley Award Symposium
Working Group on Rosins – Cannabis Analytical Science Program meeting
Analytical Solutions Forum plenaries – Food Authenticity Methods Working Group meeting – SPIFAN Working Group meeting – New Member Reception
Analytical Solutions Forum Day 2
Analytical Solutions Forum Day 1
AOAC INTERNATIONAL President Erin Crowley has just delivered the closing remarks of the 2020 Virtual Annual Meeting. “After 136 years and surviving two pandemics, we are still innovating for analytical excellence and public health.”
The Annual Meeting is over! See you next year.
AOAC’s Scott Coates, Director of the Research Institute, has just concluded his talk with the following summary:
– Surface testing for the novel coronavirus addresses a public health need
– It will provide tools for monitoring environments such as schools, hospitals, food processing plants
– It is cutting edge: This is the first Performance Tested Method for virus, the first use of in silico analysis for this area
– This Emergency Response Validation program can be used for the next public health emergency.
This final session of the 2020 AOAC Virtual Annual Meeting included three sciences discussing recent work and the challenges for detecting retroviruses in foods, water and on contact surfaces.
Infectious Viruses and Implications for Food and Food Processing Surfaces
William Burkhardt, U.S. Food and Drug Administration
It has been estimated that there are 9.4 million cases of foodborne illness annually in the US, and norovirus is responsible for 58% of those cases. Covid-19 transmission via food and food contact surfaces during the current pandemic has been an ongoing public health concern. This presentation describes reasons why transmission of SARS-CoV-2 by these vectors is unlikely and how current methodologies used for enteric viruses are applicable to Covid-19 environmental assessments.
Trusting Results: The Role of Validation, Verification, and Proficiency Testing
Yvonne Salfinger, Independent Consultant
This presentation will go over the role of test method validation and its importance, along with some examples of method performance characteristics. The need for test method verification will be also discussed, and the relevance of representative sampling and the need for validation of sampling also in quality testing. An additional quality measure, proficiency testing, will be presented.
Validation of Rapid Methods for SARS-CoV-2 from Surfaces
Scott Coates, AOAC Research Institute
The AOAC Research Institute initiated an Emergency Response Validation program for test methods that detect SARS-CoV-2 viruses on surfaces. This presentation will describe the very first use of in silico analysis in the validation of analytical methods, as well as the process to validate a SARS-CoV-2 virus detection method. It is expected that up to 8 methods will be evaluated and validated by October 2020 using this program. This process can be used for future public health threats such as influenza.
Hi, this is Marida, covering the student award-winner symposium for you.
AOAC’s Chief Science Officer, Palmer Orlandi, congratulated the young scientists after they presented their research. To learn more about their work, view the winners announcement on AOAC.org.
Hi, this is Tien with your update on the chemometrics session.
Testing for good food requires good chemometrics, say James Pyke and Dan-Hui Dorothy Yang, both of Agilent Technologies, Inc. and chairs of the session “Good Food, Beverages, and Chemometrics. ” Speakers examined chemometric approaches used with various analytical techniques as they are being applied by the food industry, regulators, and other stakeholders.
Screening techniques to detect adulteration are being developed using spectroscopic techniques, Fourier transform infrared (FTIR), and near infrared (NIR) combined with chemometric modeling. Simon Haughey, Queen’s University Belfast, noted that these techniques are gaining prominence due to their ease of use, rapidity, and minimal sample preparation with potential to be used by stakeholders in the field. He presented recent developments in the analysis of foodstuffs regarded as high risk from fraud, including adulteration of oregano and rice quality in Ghana.
As chemometric approaches to food authenticity testing and food quality analysis become more common, an understanding of the statistics and experimental designs to support these approaches becomes more urgent, says Daniel Cuthbertson, Agilent Technologies, Inc. Key factors an investigator interested in chemometric methods should be aware of are experimental design topics like the need for proper replication, capturing system variability, and different datasets to establish chemometric models and later for external validation. Methods development should focus on repeatability, and capturing analytical variability and randomization are essential for a robust model, he says. The most common statistical approaches in chemometric modeling include traditional methods like unsupervised (Principal Components and Hierarchical Clustering) analyses and supervised (Partial Least Squares Discriminate) analyses. Emerging approaches like Soft Independent Modeling of Class Analogy and Random Forrest Decision Trees develop show potential.
James Harnly, U.S. Department of Agriculture, advocated one-class modeling as a simple chemometrics approach to authenticating foods or botanical supplements. One-class modeling is a single model form of multivariate analysis using soft independent modeling of class analogy (SIMCA). Using this approach, a simple model is constructed based only on the characteristics of the authentic samples, a model is built using any commercial chemometrics platform, and the unknown sample is judged authentic or adulterated.
As food fraud becomes increasingly complicated due to the globalization of the supply chain, speakers from Agilent and Mars look to nontargeted analysis in combination with chemometrics among the most promising approaches for determining food fraud and protecting food authenticity. A study using machine learning techniques, such as random forest (RF) and support vector machines (SVM), to build classification models for authentication of rice has successfully demonstrated an empirical industry approach to tackle food fraud challenges using different analytical technologies associated with fit-for-purpose chemometric tools. This experience and knowledge could be further expanded to develop reliable and accurate models for verifying the authenticity of diverse food materials throughout the supply chain.
Hi, this is Jen with your update on the food allergen and gluten session.
Advancements in technology have allowed development of a multitude of analytical methodologies capable of detecting many allergens in a single analysis. Availability of common and standardized calibrants and incurred reference materials is needed to ensure confidence in the measurement and facilitate comparability among laboratories. This session reviewed current efforts to harmonize methodologies, paving the way for standardized methods for multiple allergen detection in difficult food matrices.
There is an urgent need for gluten reference materials for the allergen and intolerance-testing community. In Production of Consensus-Based Gluten Reference Material – and Its Challenges, Bert Popping of FOCOS GbR discussed the approach that MoniQA is taking for a consensus-based approach to source and produce such material.
The second talk, Detection and Quantification of Allergens in Foods and Minimum Eliciting Doses in Food-Allergic Individuals (ThRAll) was presented byClare Mills of the University of Manchester.
This talk was an update on the ThRAll project. The ThRall Objective is to develop a harmonized quantitative MS-based prototype reference method for the detection of multiple food allergens in standardized incurred food matrices. Mandatory labeling of allergenic ingredients has helped individuals with food allergy avoid their problem food. However, precautionary allergen labels (PAL), warning allergic consumers of unintended allergens, may be applied irrespective of unintended allergen presence. Risk-based approaches can support transparent application of PAL but require agreed reference doses for unintended allergenic protein and effective analytical methods for determining levels of unintended allergenic protein in foods.
In the third talk, Impact of Sample Preparation, Food Matrix, and Processing on Multiple Allergen Detection, Jens Brockmeyer of the University of Stuttgart discussed the impact of sample preparation, food matrix, and processing on multiple allergen detection. He talked about the basic principles of MS-Based detection methods such as protein extraction, chromatographic separation, analytical marker, specificity by MS/MS, increased specificity by multiplexing of marker for single food allergens, increased throughput by multiplexing of different food allergens (allergenic foods) in a single method etc.
Melanie Downs of the University of Nebraska-Lincoln concluded the session with a talk on Mass Spectrometry Methods to Detect Extensively Processed Food Allergens.
In addition to providing quantitative confirmation of food allergen analysis results from orthogonal methodologies, mass spectrometry (MS) methods are capable of providing critical data in situations where other methods have substantial shortcomings. In particular, food proteins that have undergone intensive and even extreme processing can be characterized and detected with MS methods. The capability to analyze allergens under these types of conditions greatly enhances the ability of food manufacturers to make data-driven decisions about allergen management practices. This presentation discussed three examples of food allergen analysis conducted in extensively processed systems: detection of milk proteins in alkaline clean-in-place (CIP) solutions, detection of cashew proteins in shared roasting oil, and quantification of soy-derived ingredients in processed foods. These three highlight the unique abilities of MS methods to help answer questions that have been challenging, if not impossible, for the food industry to conclusively answer with previous methodologies.
The increase of human salmonellosis cases over the past 10 years has triggered investigation in North America and Europe. Both the USDA and the EFSA in Europe have recently published opinions on how to better control Salmonella contamination and have highlighted the need for new technologies.
The first speaker was Bill Shaw of the USDA Food Safety and Inspection Service (FSIS) who presented on Salmonella Control Strategies in Poultry: The USDA response.
Approximately 360,000 salmonellosis cases are associated with FSIS-regulated products, triggering FSIS to implement a Salmonella Action Plan and to set new performance standards for poultry products; nonetheless, further action is needed throughout the farm-to-table continuum.
Shaw reviewed FSIS ongoing modernization activities, which include:
– Continuous FSIS lab methodology improvements: speed accuracy and dept of info from testing,
– Continuous improvement of industry affiliated labs and methods
– Collaboration with public health and research partners on Salmonella genetics
– Use of cecal data to proactively identify trends in serotype, antimicrobial resistance, etc before they are considered emergent
“We need faster testing diagnostics that support product diversion of animals and product,” noted Shaw. The US FSIS analyzes 100,000 samples each year a critical factor as they work to modernize sampling methods and pathogen screening. “We’re sort of a well-oiled machine, and new methods have to fit within the machine.”
One modernized method, implemented in 2019, is MLG method 4. It is compact, user friendly which limits errors and contamination; it has a fast lysis time, low level detection, and reduced run time from 3-4 hrs to 40-45 mins. “It can be as fast as 15 minutes for a sample with a high signal,” he noted. “For us each and every hour is valuable in our high throughput lab.”
FSIS puts its methods on the web and is expanding its Accredited Laboratory Program, as well as doing more outreach to ensure FSIS methods are correctly implemented.
The second presentation was by Marianne Chemaly of the French Agency for Food, Environmental and Occupational Health & Safety (ANSES), who discussed Public Health Impact of Salmonella in Poultry Flocks.
She discussed strategies and trends in Salmonella zoonosis and foodborne outbreaks, with a focus on the top 5 serotypes. More than 91,000 salmonellosis cases are reported each year by the European Union Members States, with probably €3 billion yearly economic burden. Salmonella spp. is in the top two of the zoonotic agents creating foodborne outbreak in Europe, together with Campylobacter spp.
Chemaly described the European Commission’s integrated “farm to fork” approach which includes risk assessment (data collection, analysis, and recommendations) and risk management (legislative measures and targets for reduction), both supported by timely and effective risk communication.
The integrative approach for Salmonella focuses on primary poultry and pig production, as the highest levels of Salmonella-positive samples occurred in meat products. However, Salmonella is carefully tracked in other productions such as milk and dairy products, vegetables, etc. The data are reported to the European Food Safety Agency by the EU member states, with the objective to adapt the legislation requirements for better and relevant control measures in both, primary and food production.
In the final presentation, Catherine Carrillo of the Canadian Food Inspection Agency presented From Thousand Bacterial Genomes to New Routine Testing Methods: The Possible Road Map.
Next-generation sequencing technologies can now render a bacterial genome much faster and at a significantly lower cost than previously possible, leading to routine use in diagnostic laboratories worldwide. This has led to an explosion of information; for example, there are currently almost 300,000 Salmonella genomes in the NCBI Pathogen Detection database. Whole-genome sequence (WGS) information can be leveraged to develop and validate routine test methods used in food microbiology diagnostic laboratories. In the past few years, CFIA laboratories have transitioned to the use of genomic data for strain typing and to infer Salmonella phenotypes such as antimicrobial resistance and serotype. Carillo described the insights gained in working with WGS as:
· WGS-based characterization of foodborne pathogens is cost-effective, reliable and more comprehensive than traditional methods
– Genomic data can and should be used to inform the development of improved methods for food testing
– WGS can be applied to the development of more rigorous validation standards ensuring better performance of the next generation of food testing methods.
Hi, this is Marida, reporting out for you on the CBD/Hemp sessions.
This session, chaired by Erin Crowley, President of AOAC and Chief Science Officer of Q Laboratories, brought together industry, regulatory, and standards development perspectives of this new industry.
President Crowley introduced the session with an overview of where we are and how we got here. Following the passing of the 2018 Farm Bill removing CBD and Hemp from the Controlled Substances Act, the industry has seen an exponential increase in product development. For those in this industry, quality control and analytical accuracy is an essential component in protecting the health and safety of the consumer in this emerging market. As regulations evolve, and as research interest in these analytes expand, it is important to have harmonized standards developed and robust analytical methods in place that are capable of meeting those needs. This session will present the current state of analytical test methods and present examples of how industry manufacturers of these products are ensuring quality from seed to sale by method development and partnerships with expert laboratories.
The industry perspective was presented by Jeff Moore and Rusty Sutterlin of Socati International in a talk entitled Challenges from the Perspective of Industry Leader of Cultivation of Seeds and Quality Control of Products.
Sutterlin reviewed Socati’s activities. Socati’s hemp seed production is a research-based process to provide customers and growers with seeds which produce plants yielding consistent phenotype, potency, and quality.
“It all begins with good genetics” noted Sutterlin. “You need good seeds to grow good plants, then you need great farmers in your supply chain. Then there is the manufacturing & technology – All require analytical chemistry.”
Jeff Moore discussed testing challenges and Socati’s lessons learned. “Testing is critical to safety and consistency of final products. Socati is trying to normalize results. They compared testing with two HPLC methods for cannabinoids using different standards and kits. They also sent the same sample to four labs. Results clearly indicated the importance of homogenized samples.
On-site quality testing with modern and validated methods is preferred, but technologically and economically restrictive for most. Use of commercial testing laboratories for final product release and customer confirmation is wrought with challenges. Developed and validated methods and harmonization of standards and testing methods among is essential.
For organizations looking to choose an outside laboratory, he had three recommendations:
– The lab must have method validation documentation,
– It must have standard operation procedures outlined,
– Before choosing, send a pre-tested sample for comparison.
This was followed by Andrew Hall of Green Scientific, who presented on Method Development: Current State and Unmet Needs.
“Cannabis is a chemical factory producing a lot of unique and valuable chemistry,” he noted, but it is well known that the marijuana plant is a difficult matrix on its own, with significant heterogeneity of chemical constituents within the fiber, seed, and flower producing parts of the plant. Cannabis varietals look very different, have different flavanoids and expression of cannabinoid chemistry. Processing includes producing crude extract, which is further isolated into CBD, CBG, etc. and potentially further processed into enriched botanical extracts which are higher in CBD. All test differently. With thousands of different products testing is a technical challenge and it is Critical to talk to your lab and work out what are the kinks, how accurate do these tests need to be.
Most jurisdictions in the US, Canada, and Mexico have settled on testing for an array of potential contaminants, including pesticides, mycotoxins, microbiological indicators and pathogens, gross contaminants, and heavy metals. In the absence of federal guidance, laboratories have had to develop and validate their own methods. There are many accounts of laboratories producing starkly different potency measurements for the same products—some results varying by as much as 40 percent.
In the third talk, AOAC President Erin Crowley of Q Laboratories presented on the Role of CASP and AOAC Standards Development.
AOAC’s Cannabis Analytical Science Program (CASP) was formed to develop the consensus-driven standards and methods needed to promote accuracy in label potency claims and to address public safety issues. CASP is one of several areas where AOAC has demonstrated its process is effective. Crowley reviewed current working groups, standards and Official Methods approved to date, and future activities.
“What can you do? Get involved,” she advised. She noted that CASP is a balanced group with industry, academia, and government, offering opportunities from contributing financially to contributing expertise. For businesses, contributing positions you as a leader in your industry.
Crowley summed up how AOAC standards & methods development, laboratory proficiency testing, Official Methods of Analysis, and publications come together for a complete and harmonized quality system through analytical excellence.
In the final talk of this session, Brad Kelly of Socati spoke on Industry Perspective: Looking to the Next Phase and Associated Challenges.
The burgeoning hemp industry now has established industries that are demanding quality and consistency along with modern certifications and process documentation. Socati is leading this industry by producing natural, hemp-derived ingredients that feature fully customizable cannabinoid profiles, raising or lowering the levels of CBD, CBG, CBN, and several other minor cannabinoids. This gives manufacturers complete control over what they put in their products and enables them to serve the needs of a broader range of consumers.
The Socati ecosystem:
– starts with genetics – if molecules aren’t there in the right proportion, we will not get the products we are looking for.
– purification and THC remediation – since people want nondetectable THC
– organic extraction – a huge focus for consumers.
As a business, hemp offers many opportunities:
– popularity of infused products – consumers are interested in CBD and other cannabinoid improved products. In the last few years the consumer profile has expanded into all demographic groups
– there is a growing body of research on cannabinoids and their properties; with a lot more science out there to support the safety and efficacity of these products to help quality of life
– “FDA approval is the 900-pound gorilla: when they cough we worry about getting a cold.” He concluded. “We need FDA to come down with some positive, difinitive guidance to provide stabilty and opportunities the industry needs.”
Socati’s products include USDA certified organic hemp extracts; “defined spectrum oil” where Socati’s technology allows them to “dial in” the ratios so people get the profile they want; defined spectrum water dispersible distillate; flavored 10mg dose powder packets; gummies, softgels, capsules, pressed tablets, and the traditional tinctures.
Socati has a private label program – they manufacture for other companies; their goal is to be the “trusted, traceable and transparent supplier.”
Challenges in Setting Probiotic Quality Standards
Presented by Charles Budinoff, DuPont Nutrition and Biosciences
As the number of probiotic products available to consumers grows, so does the need for robust testing methods to determine quality and content. Human clinical research on probiotics demonstrates that specific strains and targeted doses are essential for efficacious outcomes. Probiotic consumers trust manufacturers to provide high quality products, and without up-to-date and relevant standards and methods for proving quality, the industry is threatened by products that may not contain the claimed probiotic strains and quantities. Traditional agar enumeration methods have long been used as the gold standard for evaluating probiotic cultures but are labor-intensive, pseudo-selective, and have a high degree of variability. Various DNA methods for probiotic identification, some of which are inexpensive and quick time-to-results, have been developed and are now publicly available. How best to enumerate probiotics is still under debate, but new methods, such as digital droplet PCR, are showing promise and are strain-specific and high-throughput. In this session, we will explore the work being done by several key stakeholders in probiotic quality and discuss the value and challenges of new testing methods.
Coffee and Testing: From Bean to Cup
AOAC’s Dawn Fraser is interviewing Mark Corey of the National Coffee Association.
Corey noted that testing is both challenging in coffee and important, as consumers are interested and have a stake in coffee’s characteristics such as demonstrated health benefits, potential pesticide residues, and fraud. “Being able to analyze is crucial to being able to protect consumers,” he said.
In the food fraud area, this is largely an issue of the cost differential between Robusta and Arabica coffees. With high-end coffees marketed as 100 percent Arabica, both fraud and accidents can happen. Coffee is a high value-added product, which opens opportunities for unscrupulous sellers to cut Arabica with the much cheaper Robusta. In last few years, the coffee industry has conducted extensive research to identify ways to distinguish the two species. This is complex, since scientists believe Arabica evolved from Robusta and there has been extensive hybridization; hence, the molecular fingerprints are similar. Robusta has up to twice the caffeine of Arabica, but if small quantities are added, it is not easily detected.
While highly skilled human tasters can detect down to 5 percent Robusta in Arabica, smaller adulterations cannot be detected this way so in the last few decades, the industry has been looking for an identifying analyte. Looking at DNA, the issue is it is denatured in roasting. The latest approach is to look at chloroplast DNA to identify elemental speciation fingerprinting by geography – akin to the “terroir” in wine industry – through molecular fingerprints of characteristics like soil, sun, and rain. This approach has been developed and authenticated by coffee industry, but it might be valuable to standardize and validate these methods at international level.
Setting a Structured Food and Feed Laboratory Testing Capacity in the Arab Region
In this Spotlight talk, Samuel Godefroy of the Université Laval is reporting out on the current status in this part of the world, including areas like accreditation and ensuring a structured network of laboratories so that testing in this region is fast and reliable. He reviewed the mandate and mission of the EU’s RLs which include providing guidance and support to NRLs, and in the key areas of maintaining reference collections and managing proficiency testing.
In early 2020, a survey of Arab accreditation bodies, food competent authorities, stakeholders and partners was conducted to identify gaps and future areas of investments. The survey revealed that by a large margin, Arab stakeholders consider that the region has a sufficient food and feed laboratory testing capacity. Nonetheless, there are challenges including access to accreditation, performance reliability, and a shortage of competent analyts and reference materials.
Hi, this is Marida, and I am reporting out on the Spotlight talks for you this morning.
Inspiring the Next Generation of Analytical Food Scientists – Helping AOAC Make a Positive Impact
How can we engage a new generation of food analytical scientists? In this short talk, Dustin Starkey of Abbott described his research and insights into what drives young scientists to join or leave an association like AOAC, how to reach them, and what value they are looking for in an association experience. Looking at several personas from new graduates to young professionals and faculty, Dustin broke out some take away lessons:
– For graduate students: “Jobs and social are huge.”
– For young professionals: “Career advancement and development and opportunities to volunteer are critical.”
– For young faculty: “Strong science, impactful mission, and opportunities for students.”
How does AOAC rate in its outreach to young scientists? Starkey’s interviews with young stakeholders revealed that AOAC’s strengths are its scientific credibility and methods; but the organization has low brand awareness (even by those who know of AOAC methods) and limited programming for students. Moreover, AOAC’s perceived mission of method development can be seen as uninspiring. Also, a key area of interest to researchers, securing research funding, is not part of the mission.
But Starkey identified a huge and relatively easy win: student competitions were mentioned as a powerful incentive by almost all survey respondents.
Hi, this is Dawn, and I have summarized the food fraud session for you below.
Adulteration of foods is one of the oldest problems in the food production process. While inadvertent contamination/adulteration can generally be addressed by implementation of good manufacturing/agriculture practices, the intentional adulteration of foods is a more complex problem. Different countries have historically had to deal with this issue on a local level but the nature of present day international trade practices requires an approach that requires international cooperation and information exchange to fight it. The authors discussions covered:
Approaches Used to Assess the Quality and Authenticity of Fruit Juices in Europe and the Importance of Standardized Methods – Presenter Mikko Hofsommer
Nikko discussed quality issues in fruit juices and methodology that can be used to detect it. His presentation particularly covered the use of SNIF NMR to detect the addition of sugars from adulterants such as beet sugar in juices such as apple and orange juice.
Overview of AIJN Code of practices
David Hammond (for Dana Kreuger) discussed:
– Covered AIJN code of practice reference guides
– COPEG- Expert committee made up of 20 experts from industry, academia and juice laboratories.- Develops reference guide to cover criteria for experts to use to determine authenticity of juices. Described how these parameters were set and/or adopted from present regulations if available (ex. Brix values for juices).
Approaches to Detect the Adulteration of Juices Using Chromatographic Methods- Ramin Jahromi
The presentation highlighted some of the more significant approaches including the use of coumarins and psoralens, which have proved very useful as a means to differentiate between lemon, lime and ad-mixtures of these juices.
Detecting Adulteration of Lemon and Pomegranate Juices- Mike Farrow
– Use of SCIRA
– Titratable acidity (Set by FDA standard of identity)
– Brix values
FDA Regulation of Color Additives in Foods- Bhakti Petigara
– Purposes of food coloring and color additive requirements/Permitted colors in the CFR
– Discussed how a color additive is approved.
– Industry shift to food colors from natural sources.
FCC Identity Standards- Gina Clapper
– Food Chemicals Codex – How to recognize a good ingredient standard.
– Validated testing required to ensure product quality.
– 1200 individual monographs
– Identity Standards proposed for foods like honey.
– FCC Forum Online- public comment portal
– Future Plans: Honey expert Panel, Olive Oil Authenticity
Hi, this is Marida, and I have summarized the vaping session for you below.
Analytical Strategies to Characterize Products Intended for Inhalation After High-Temperature Vaporization Vaping products have been developed without appropriate regulatory oversight and, as a direct result, thousands of people have developed serious respiratory illnesses and at least 47 people have died. Recent events and media attention have precipitated proposed legislative actions including product bans which have been proven to simply drive consumers to more dangerous black market sources.
Session Chair Matthew Noestheden of Supra Research and Development introduced the topic by noting that there is an analytical gap that AOAC is well positioned to provide leadership in filling. Presenters from Supra Research & Development, the US National Institute of Standards and Technology, the U.S. Centers for Disease Control and Prevention, the Maryland Medical Cannabis Commission, and manufacturers Dosecann LD Inc. explored current approaches to evaluating vaping products to determine how AOAC consensus methods could play a role. In the five talks, we heard:
– how the high temperatures of vape pens can generate unexpected and potentially dangerous chemical agents, and what methods are effective for identifying “vaporization potential”
– the purity and stability of commercially available vape fluid products and the evolution of byproducts during storage, heating, vaporization, and combustion.
– how corrosion of the internal metal components of e-cigarettes produces particles in the aerosolized liquids inhaled by consumers
– a regulator’s view of how consistent testing standards are slowly becoming available for industry use, but the industry is outpacing the science
– a vape product manufacturer’s story including the process and analytical safeguards involved in turning cannabis biomass into vape products with a cannabinoid concentration of around 90%
Hi, this is Tien, and I have updated the blog on the PFAS session for you below.
PFAS, environmentally persistent man-made chemicals widely used in industrial processes and consumer products, can lead to environmental contamination, may cause serious health conditions, and are, therefore, of public health interest. In response, U.S. federal agencies, including USDA, CDC, EPA, and FDA, have developed PFAS analytical methods to address specific targeted needs within their respective agencies. Due to the widespread use of PFAS, background levels as well as the various matrices of concern by federal agencies present unique analytical challenges. Representatives from federal agencies outlined various sample preparation and determinative techniques developed.
Emilio Esteban, U.S. Department of Agriculture, reported that USDA recently developed—and currently uses–a method that screens, confirms, and quantifies 16 PFAS compounds in beef muscle and blood plasma, using methanolic extraction followed by UPLC-MS-MS. “We needed a method to monitor the beef supply for PFAS that uses quick and simple extraction and delivers rapid and reliable results,” he said. The method is available publicly on the FSIS website as part of the FSIS Chemistry Laboratory Guidebook: https://www.fsis.usda.gov/wps/wcm/connect/365c4eb9-cab2-4ef4-b9f3-b8d1cdb87241/CLG-PFAS-2.01.pdf?MOD=AJPERES
CDC has developed analytical methods to quantify select long- and short alkyl-chain and alternative PFAS in human specimens. These methods use isotope dilution on-line solid-phase extraction liquid chromatography-tandem mass spectrometry. Although measurements can be made in both urine and serum, studies show that serum is superior for biomonitoring of PFAS. The method is highly selective, accurate, and precise for trace-level quantification of PFAS. The CDC methods have been used to assess PFAS serum concentrations in the U.S. general population through the National Health and Nutrition Examination Survey since 1999.
U.S. Environmental Protection Agency (EPA) has analytical methods in various stages of development for PFAS in drinking, ground, surface, and wastewaters in addition to solid samples such as soils, sediments, biosolids, and tissues. Protocols for sampling and analysis of air emissions are being developed. The EPA is also developing and evaluating methods for total organic fluorine, total oxidizable precursors, and nontargeted analyses. Currently, there is no EPA-approved method for PFAS in fish tissue, and EPA uses commercial labs’ proprietary methods for this matrix. A high priority for EPA is total organic analysis using combustion ion chromatography, possibly a screening technique.
FDA, leveraging its Total Diet Study (TDS) in 2018, developed a Quick, Easy, Cheap, Effective, Rugged, Safe (QuEChERS) extraction method for PFAS in a wide range of food matrices (produce, dairy, meat, and bread samples), with analysis by LC-MS. During method development, challenges arose with matrix suppression, interferences, false positives, and method blanks. FDA optimized the single-lab validated method with improved chromatography and additional cleanup steps. The agency plans to add new matrices, which may require further method optimization.
While most water samples fall within EPA jurisdiction, bottled water lies within the scope of the FDA. The FDA Office of Regulatory Affairs, Arkansas Laboratory verified EPA Method 537.1 for PFAS determinations in bottled water samples, including a comparison of detection limits determined on two separate instruments and results of determinations performed on well water on an onsite water treatment facility.
These methods will allow federal agencies to continue monitoring PFAS compounds in the U.S. food supply and environment.
Targeted and Non-Targeted Methods for Comparing Botanical Preparations
Botanical dietary supplements represent diverse materials ranging from plant materials to crude or refined extracts to enriched or single phytoconstituents. This enormous bandwidth of materials, paired with the wide range of analytical methodologies available, provides the analyst with an overwhelmingly complex network of choices when comparing and/or evaluating botanical preparations.
This presentation, by Guido Pauli of the University of Illinois, looked at three key questions related to the use of targeted vs. non-targeted methodology: 1) why botanical identity and authenticity are important; 2) why botanical adulterations occur; and 3) how targeted vs. untargeted methodology can address identity, authenticity, and/or adulteration.
Kratom (Mitragyna speciosa): How Do You Approach the Standardization of Emerging Herbs?
Standardization is the nuts and bolts of how we measure things. If you consume an herb and you take medication, there may be an interaction. In practice this is seen in the stickers pharmacies put on medications, such as “Do not take with grapefruit.”
This session, presented by Nicholas H. Oberlies of the University of North Carolina, discusses how to determine if there is potential interaction between drugs and supplements. He illustrated the topic by looking at the herb Kratom, used both for pain relief and to treat opioid addiction. Its popularity is illustrated in Greensboro North Carolina, where you can find at least three “Kratom bars.”
Hi, this is Jen, and I am summarizing the Dietary Supplement sessions for you.
Dietary Supplement Analyses to Support Population Exposure Estimates
In the first talk of this session, Karen Andrews of the U.S. Department of Agriculture described a project to evaluate the feasibility of obtaining reliable estimates of constituents in dietary supplements.
Dietary Supplements are popular in the US and there are more than 80,000 dietary Supplements available through this a multi-billion dollar industry. She discussed how this impacts health, given that epidemiological studies of nutrient intake and health associations use the manufacturer’s label as the source of information for the content of dietary supplements. However, dietary Supplement Ingredient Database (DSID) results indicate that labels usually underestimate vitamin and mineral content in multivitamins, up to an average of 30% for some.
Hi, this is Dawn, and I am summarizing the PCR Quantification sessions for you.
This session included the following talks:
– Challenges of PCR Quantitation – and Possible Solutions – presented by Bert Popping of FOCOS GbR
– New Reference Material – To Overcome Problems in PCR for Low Copy Number Target Gene presented by Kazumi Kitta of the National Agriculture and Food Research Organization
– Never Miss Low Copy Number DNA Molecules in PCR Testing! – New Reference Material for the Detection of Animal Species presented by Riztyan Ian of Fasmac Co., Ltd
– Optimization of PCR Workflows for Accurate and Sensitive Quantification of Nucleic Acids, presented by Yann Jouvenot of Bio-Rad Laboratories
While detection is often reasonably sensitive, quantification can present a significant issue. Not knowing the composition of the sample (e.g., 50% muscle, 20% liver, 30% connective tissue) will make it impossible to accurately determine and difficult to estimate the quantity of tissue from an animal present in the sample. The session covered different cases and possible solutions.
Polymerase chain reaction (PCR) quantitation in the field of GMO, animal and plant speciation and food allergens is common practice in laboratories since it is a comparatively rapid and cost-efficient method. PCR is extensively used for molecular diagnostics and detections as a gold standard. There are no measures to assure the performance of PCR analysis at a low copy number, such as a single-digit number level. For resolving such problems, a novel reference material was developed containing a defined copy number of target DNA and can be used for evaluating the quality of analytical factors such as instruments and reagents as well as for generating an accurate standard curve, which will serve for more reliable data production.
Accurate animal species detection is important to assure food ingredients comply with certain regulations such as related to allergen or halal. In the latter case of halal, pork, and pig derivatives are prohibited so porcine contamination is critical in halal food productions. Food testing laboratories require DNA reference material that is specifically designed and works effectively for low copy number of DNA to provide an accurate analysis. In this session, speakers demonstrated the application of a new reference material in detecting low levels of porcine DNA by qPCR. Analysis of qPCR amplifications at low copy number of porcine DNA molecule were presented and discussed.
PCR and its derived technologies, quantitative PCR, and digital PCR (qPCR and dPCR), have revolutionized molecular biology and their applications have since extended to many other disciplines. While kits for dedicated applications have multiplied and streamlined, PCR and software progress have made the analysis of the data a basic understanding of the workflow necessary to obtain reliable data. The final presentation outlined the basic steps of a qPCR workflow: experimental design, assay design, sample preparation, qPCR, and data analysis. The main points of consideration will be discussed at each step, in order to provide guidance for the successful use of the technology.
Preliminary Evaluation of Commercially-Available Ergot Alkaloids Kit
The Canadian Grain Commission monitors ergot alkaloids in Canadian grain by ultra-high performance liquid chromatography-tandem mass spectrometry. This analytical method allows them to obtain concentrations of each of the individual EAs (ergocornine, ergocristine, ergocryptine, ergonovine, ergosine, ergotamine) and their epimers.
Recently, ergot alkaloid kits have become commercially available. In this talk, Kerri Pleskach of the Canadian Grain Commission presented a preliminary evaluation of two of these, one ELISA and the other a lateral flow device. They compared results of the LC-MS/MS versus the kits using 11 samples where they extracted 1 test portion per sample per day, ran 2 aliquots, repeated this for 3 days, and ran control standard, blank and IHRM per day per kit. Discrepancies were noted, some of which could be the result of cross reactivity. Although work has been paused due to Covid, the team plans to finish analyzing 29 wheat and CWAD samples, determining accuracy and precision, and determine cross reactivity of each ergot alkaloid.
In Multi-Mycotoxin Analysis Using LC-MS/MS and LC-HRMS, Jon Wong of the U.S. Food and Drug Administration described a comparison of two multi-mycotoxin methods involving liquid chromatography equipped with low resolution triple quadrupole mass spectrometry (LC-MS/MS) and high-resolution quadrupole-Orbitrap mass spectrometry (LC-HRMS) to analyze finished cereal and nut products for 26 mycotoxins. He concluded that both platforms have their advantages and disadvantages; procedures to optimize the performance of LC-MS/MS for target analysis are well-established and characterized but are unable to detect unexpected compounds. Although LC-HRMS was demonstrated to be reliable for quantitative purposes using targeted acquisition modes, it is more challenging to use than LC-MS/MS. However, LC-HRMS has expanded capabilities to perform non-target acquisition analysis that are better suited for screening purposes.
Hi, this is Marida, covering the Ergot Alkaloids session for you this morning.
This session kicked off with an introduction on “ergot” the disease, the variety and chemistry of ergot alkaloids, and regulatory activities by Sheryl Tittlemier of the Canadian Grain Commission.
The first presentation looked at the grass parasitic fungus Claviceps purpurea sensu lato, which produces sclerotia with toxic ergot alkaloids and uncharacterized indole–diterpenoids. In “Diagnostic Fragment Filtering for Unravelling the Ergot Alkaloid and Indole–Diterpenoid Metabolome in Claviceps purpurea sensu lato,” Silvio Uhlig of the Norwegian Veterinary Institute described a study to tentatively identify as many peptide ergot alkaloids and indole–diterpenoids as possible using LC–HRMS and the built-in diagnostic fragment filtering tool in MZmine 2 for data extraction. The sample set consisted of 66 Claviceps sclerotia from Southeastern Norway and Saskatchewan, Canada, including both wild grasses and important cereal grains such as rye. He concluded that:
– DFF is a valuable tool for MS data extraction in “semi-targeted” metabololomics studies
– Ergot sclerotia contain many more than the 12 “major” ergot alkaloid congeners, but these “major” congeners likely account for at least 50% of the toal ergot alkaloid content
– Certain indole alkaloid analogues could be used as chemotaxonomic markers for species within C. purpurea sensu lato.
Hi, this is Tien, covering the final session for you this afternoon.
Naturally occurring elements like arsenic and nanoparticles, found in staples such as rice and infant formula, respectively, can be potentially toxic at trace levels. But with novel methods and advances in technology, scientists can detect for potential contamination at even very low concentration levels. In the scientific session, “Novel Methods for Contaminants,” speakers fromleading technology providers focused on different materials or substance classes that are of increasing global food safety or environmental concern. As such, these products are likely to be found in regulations and must be often identified, characterized, and quantified as impurities in different matrices–leading to a high demand for accurate standards and robust analytical methods.
Speakers touched on nano- and microparticles, marine biotoxins, polyfluorinated alkylated substances (PFAS), and elemental impurities. In “Certification of Marine Toxins by Quantitative NMR (qNMR) and Isotope Dilution MS (IDMS),” Markus Obkircher, MilliporeSigma, explained the proper characterization of such materials for the intended use as certified reference materials in quantification experiments.
Other presentations highlighted the development of suitable methods for sample preparation, and detection and quantification of the mentioned contaminants, as well as the validation of these analytical methods. Analytical techniques applied for these purposes include, among others, LC/GC-MS, isotope dilution MS (IDMS), quantitative nuclear magnetic resonance (qNMR), and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS).
Lately, there has been growing interest in the analysis of PFAS compounds as trace amounts have been found in groundwater. In “Determination of PFAS Compounds Using Tandem Liquid Chromatography-Mass Spectrometry (LC-MS/MS), William Lipps, Shimadzu Scientific Instruments, described development and validation of a method to determine PFAS in water samples and solid samples, including biosolids and soil.
While rice is an extremely important dietary source all over the world, it also contains harmful elements such as arsenic, which can be taken up from the soil. Traditional elemental analysis involves digestion of the rice grains, which only gives an average value per rice grain. In “Elemental Imaging of Different Types of Rice Using LA-ICP-MS,” Derrick Quarles and Ciaran O’Connor of Elemental Scientific proposed that laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is a technique that can offer spatial resolved elemental images of rice grains.
Quarles also focused on elemental/inorganic content of arsenic and its effects on flavor, color, and aroma of wines in “Elemental Analysis (Total and Speciation) of Wines from Various Regions of the World.” Analytical testing is an important aspect for determining the quality of the wine from the perspective of food safety.
Hi, this is Jen, covering this session for you this afternoon.
The role of reference materials is vital to AOAC’s Official Methods programs, but the process for selecting (or developing) a reference material can be unclear. This symposium discussed the various stages of standards development in the AOAC programs and how reference materials play a key role in every step.
A Call for Experts! How CASP Working Groups Select Reference Materials in the Standard Development Process
After a welcome from Pat Bird on behalf of AOAC’s TDMR, Julie Kowalski of JA Kowalski Science Support LLC introduced the AOAC Cannabis Analytical Science Program and pointed out some key reference material challenges in the cannabis industry:
– This is still a young industry
– You can’t legally ship high THC samples across state lines
– Cannabis is new to reference material suppliers. They need to understand what we need and how to adjust on the fly as regulations change
– There are no standard reference materials in matrix material. Hemp is the first one and it is still being worked on by NIST.
Her conclusion? Working Groups need to focus on how to do work and still be flexible.
In Strain Characterization and the Role of Reference Strains in Microbiology Method Validation, Maria Nelson, AOAC Technical Consultant discussed the Micro Method Validation process. Some takeaways: We don’t have Standard Reference Material but, we do have strains that are from reference sources. That is important because you want to know what you’re testing is what you are testing and how the strains are characterized. We can look at genome, biochemical methods, color changes, films etc. all to give a profile. We can even go old school and do Gram-stain. Well characterized assays need well characterized strains to accurately detect microorganisms in food and environmental samples.
In Strategies for Analytical Method Validation when Reference Materials are Unavailable, Beth Mudge of the National Research Council, Canada discussed strategies for chemical and analytical methods when you don’t have reference materials. Reliable measurement results require traceable values with uncertainties (reference materials)
In An Inside Look at Expert Review Panels Evaluation of Reference Materials in the Validation Process, Donald Gilliland of Abbott Nutrition discussed what SPIFAN is and the pathway from candidate methods through final action methods. Don also talked about how the ERP review the data in the candidate methods. SPIFAN started about 12 years ago. Beginning in 2008 met in Dallas had a small room and they had to keep bringing chairs into the room. 2010 Orlando was the first Stakeholder Panel meeting. Why was SPIFAN initiated? There was a recognition that new standard methods were needed. CODEX, AOAC ISO methods were outdated, no longer fit for purpose. Many of the methods were validated using limited infant formula or adult nutritional products. Standard methods were not even available for use. There were discrete gaps for certain nutrients. Needed to identify reference material for the purpose of evaluating these methods.
Hi, this is Marida, covering the Annual Meeting for you this morning.
After a delayed start, the AOAC Working Group on Glyphosate in Food Matrices just concluded a zoom meeting in which they solidified the scope of the working group, what expertise is needed in the Advisory Panel, and what the milestones of the work will be.
The first step will be developing one or more SMPRs for the simultaneous determination of glyphosate (including glyphosate trimesium) and all its metabolites: N-acetylglyphosate, aminomethylphosphonic acid (AMPA) and N-acetyl-aminophosphonic acid (N-acetyl AMPA).
After extensive discussion of the matrices to be covered by the project, the Advisory Panel agreed on the following list:
– coffee beans, teas, carobs, hops, spices, and herbal infusions;
– High water content matrices (stone fruits, leafy vegetables, potatoes, watermelon, beets);
– high fat (tree nuts, oil seeds, oily fruits and derived products);
– dry commodities (soybeans, lentils, yellow peas, chickpeas, wheat, corn, barley, oats, rice; and
– genetically engineered crops.
These may be further refined but the Working Group is planning to start development of the SMPRs in October.
As the interest in food safety grows, the characterization of trace elements in foodstuffs is of increasing importance. Consequently, there has been an increasing number of regulations that place restrictions on the maximum allowable concentrations of certain elements in food. In recent years, a number of methods have also started to characterize the presence of certain chemical species and nanoparticles in food samples as knowledge of the potential toxicity of these factors are gained. This session covered a wide range of topics discussing the presence and concentration of a variety of different elements, the speciation of metals and the characterization of nanoparticles in foodstuffs and cannabinoids.
Is Elemental Speciation Important for Analysis of Foodstuff?
In this presentation, Andrea Raab of the University of Aberdeen gave several examples of why speciation is of interest to the consumer and to the food industry. With some elements, certain species are known to be more toxic than others. Other elements are beneficial when present in certain molecular forms but of no consequence or even toxic in others.
Trace Metal Analysis in Cannabis Using Inductively Coupled Plasma Mass Spectrometry and the Impact of varying Matrices on Spike Recovery
Inductively coupled plasma mass spectrometry (ICP-MS) can measure trace amounts of elements in a variety of matrices and is now the primary technique to determine heavy metals in cannabis. In this presentation, Kevin Smith of Naproresearch presented the methods used and validation data for measuring cadmium, arsenic, and lead from 0.5 to 0.02 ppb and mercury from 0.05 to 1.0 ppb in Cannabis flower and distillate, and discussed a variety of other cannabis matrices as well.
Characterization of Silver Nanoparticles in Dietary Supplements by Single Particle ICP-Mass Spectrometry
Nanomaterials containing metals are increasingly being used in consumer, industrial, and medical products and are subsequently being released into the environment. Methods for detecting, quantifying, and characterizing these materials in complex matrices are critical to understand their effect on environmental quality and human health. This presentation by Aaron Hineman of PerkinElmer described Single Particle Inductively Coupled Plasma Mass Spectrometry (SP-ICP-MS) as a metrology tool in assessing the fate of engineered Nanoparticles in complex aqueous samples.
In Analysis of 16 Elements in the Top 10 Most Consumed Seafoods in the US, Sean Conklin of the U.S. Food and Drug Administration presented the results of analysis of a representative sample set for total arsenic as well as 15 other elements using a U.S. Food and Drug Administration validated method (for Cr, Mn, Ni, Cu, Zn, As, Se, Mo, Cd, Hg, Pb) which has recently been single-laboratory validated for an additional 6 elements (V, Co, Sr, Sn, Tl, U).
Genomic, Proteomic, and Microbiological Methods for Probiotics Analysis
This session, presented by Quanyin Gao of Herbalife, discusses the identification and quantitation of probiotics, along with challenges and solutions. The industry must advance their techniques to identify and appropriately analyze these ingredients. Proper identification of probiotic materials is important for establishing quality control standards lack of them can result in a potential adverse health risk. It is also important to accurately identification the strain level in probiotics. The analytical methods currently available have faced challenges for accurate quantitation of different formulations and stability studies.
Hi, I’m Jen and I will be covering the Probiotics presentations for you this afternoon.
As the probiotic market expands, with its significant opportunities for improving human health, analytical methods are increasingly important to the nutritional industry for establishing quality control standards and to avoid misidentification or lack of identification that can result in a potential adverse health risk. Many strains of bacteria that provide a health benefit, like E. coli Nissle 1917, are defined as probiotics, but alternate strains of the same species, such as the notorious E. coli O157:H7, pose a health threat. This session included presentations from industry and organizations on the challenges and solutions to identification and quantitation of probiotics.
A Multilaboratory Study Utilizing nDATA (non-target Data Acquisition for Target Analysis) Workflow for Multiresidue Pesticide Screening by Ultra-High Performance Liquid Chromatography-High Resolution Mass Spectrometry with a Compound Database
This talk, by Jon Wong of the U.S. Food and Drug Administration, reviewed a complex project he and two others undertook where 28 laboratories screened for 51 pesticides in 10 high moisture fruits and vegetables using an nDATA (non-target Data Acquisition for Target Analysis) Workflow. The study demonstrated the use of UPHLC-HRMS for screening pesticides and the workflow was found to be easy to implement, cost effective and practical for screening purposes, especially for a large group of pesticides.
Dioxin and PCBs Analysis in Food and Feed Using GC-HRMS According to the Most Stringent European Regulations presented by Gian Piero Luciani of Tentamus Agriparadigma S.r.l. focused on the analysis of dioxins and PCBs in relation to European legislation. This talk highlighted the differences, advantages, and disadvantages betwen high- and low-resolution mass spectrometers.
Exact Masses for Authentic Food – What Can Proteomics Do for Food Authenticity?
The authenticity of food is a major quality and safety concern worldwide. The mass spectrometric characterization and quantitation of proteins in food, also known as Food Proteomics, has become a very useful and versatile novel tool to address authenticity issues. In this talk by Jens Brockmeyer of the University of Stuttgart, the methodological basics of Food Proteomics were discussed, with several examples including identification of markers for shellfish allergens, which are found in other foods as well. Marine foods are major targets of fraud because of the significant differences in price and the incredible complex species diversity.
Using High-Resolution Mass Spectrometry to Detect and Investigate the Fraudulent Adulteration of Oregano
The herbs and spices sector is particularly affected by this issue of adulteration with a study showing around 25% oregano sold has been adulterated with olive leaf. A methodology based on marker discovery employing LC-HRMS data with subsequent transfer of these markers to LC-MS/MS with rigorous in-house validation proved to be an efficient strategy in the development of simplified MS-based approach to address the problem of oregano adulteration. Another study investigating oestrogen-like activity in oregano extract with the help of LC-HRMS will also be presented as well as the latest development to a faster methodology to address food authenticity based on LC-HRMS and chemometrics.
Tattoos and permanent makeup have greatly increased in popularity over the past several decades. These types of body art are produced by injecting tattoo inks containing various pigments through the epidermis into the dermis of the skin. Globally, the safety of tattoo inks has been a subject of interest and has prompted the consideration of regulatory requirements for the tattoo inks as well as their pigment components. Development of analytical methods to determine the composition of the many types of tattoo inks available in the global marketplace has been challenging and complex. This symposium spoke to the challenges for tattoo inks on both the regulatory and analytical fronts. Presentations included:
EU Regulation on Substances in Tattoo Inks and Permanent Make-Up presented by Ana Maria Blass Rico and Giuseppina Luvara of the European Commission
Investigations on Photodegradation Products of Pigments Used in Tattoo Inks presented by Urs Hauri of the State Laboratory of Basel-City, Switzerland
Determination of Primary Aromatic Amines (PAAs) in Tattoo Inks with Different Methods Using GC-Q-ORBITRAP presented by Flavio Ciesa of the Italian Provincial Agency for the Environment and Climate Protection
Tattoo Pigments and Inks: Regulatory Challenges and Overview of Analytical Methodology presented by Marianita Perez-Gonzalez of the U.S. Food and Drug Administration
Development of Non-Targeted Methods for the Analysis of Tattoo Inks presented by Christine M. Fisher of the U.S. Food and Drug Administration
Evaluation of an Automated Sample Preparation System for Mycotoxin Analysis in Foods
Kai Zhang of the U.S. Food and Drug Administration discussed his team’s development and evaluation of a straightforward and automated sample preparation procedure for LC-MS-based multi-mycotoxin analysis. This workflow integrates off-line devices, such as centrifuge, shaker, liquid and solid dispensing units, into a unified platform to perform gravimetric and volumetric dispensing, capping/decapping, extraction, shaking, filtration and centrifugation. Two robotic arms provide sample transportation without human assistance. This platform is intended to replace manual operations and significantly increases the degree of automation and standardization for sample preparation.
Analytical Challenges and Approaches for the Determination of Vitamins in Encapsulated Forms in Supplements and Foods
“Chemistry is king, but communication is vital,” said Walt Brandl of Merieux Nutrisciences in his presentation on challenges and solutions in the analysis of encapsulated vitamins.
Encapsulated vitamins are becoming both increasingly common and complex in formulations of both dietary supplements and food products and the use of lipid, proteinaceous and polysaccharide coating, sometimes used in combination, poses challenges to the analytical laboratory.
In this presentation, Brandl shared suggestions for the preparation, extraction and determination of products using encapsulated vitamins, as well as suggested changes to quality control procedures.
He concluded: “If you’re on the manufacturing side, let the lab know your source material, form of the nutrient within the encapsulation, and any formulation changes. Work with the lab; rather than the old school buyer-supplier relationship where we drop and dash the sample in the receiving area and are very surprised when the results come back inaccurate.”
Analyte Stability Issue during Sample Preparation: Recommendation for Best Practices
What storage and preparation factors can affect samples and what do we know about best practices in this key area? In the pharmaceutical industry, it has been long recognized that ensuring analyte stability is critical to accurate and precise quantitative bioanalytical methods; but in the dietary supplement area this has been neglected. During sample preparation and analysis in lab testing, the sample could be exposed to different pH, temperature, and light, variables that can cause instability. In this presentation, Aihua Liu of Dyad Labs shared best practices to assess analyte stability with different pH, temperature and light exposure as demonstrated through studies of stability factors in two cobalamins, 16 cannabinoids, and seven fat-soluble vitamins.
Techniques and Tools for Simplified Sample Preparation
Before the introduction of the highly sensitive and selective LC-MS and GC-MS instrumentation commonly used for today’s multi-analyte methods, complex compound or class-specific analytical methods were required to meet analytical requirements. These methods often involved cumbersome and time-consuming multi-step isolation and enrichment of the compounds of interest, followed by cumbersome and time-consuming multi-step cleanup.
Today, a simple extraction procedure followed by a simple cleanup step (such as pass-through SPE) can provide methodology suitable for accurate determination of hundreds of analytes from complex matrices. Of course, simplified extraction and cleanup methods are not fool-proof; co-extractables, such as water, pigments, leachates, and lipids, need to be considered to maximize cleanup and avoid recovery losses of individual compounds or compound classes. In this presentation, Michael S. Young of Waters Corporation (retired) discussed modern multi-residue analyses, in particular simplified SPE.
He concluded that effective sample preparation is still essential to overcome the challenges related to trace level contaminant analysis. Simple pass-through cleanup methods have been applied to multi-residue methods suitable for determination of hundreds of compounds in an single analysis.
Hi, this is Marida. I’ll be covering QBD, Hi Res Mass Spec, and Probiotics for you this morning.
Sample Preparation for Vitamin A and E Analysis
Selection of sample preparation techniques and operation parameters is crucial to QbD analytical method development. A good sample preparation procedure will ensure the integrity of the analytes and adequate recovery, critical to method precision and accuracy. An efficient sample preparation can also help reduce the sample test turnaround time and overall cost.
Following an overview of QbD concepts as applied to method procedures, Xun Yan of Amway Corporation used vitamins A and E analyses as an example to discuss several common sample preparation techniques and make recommendations on key essential parameters for a robust and accurate method.
Hi, this is Tien, with the final post of today’s blog.
Detection of food pathogens in routine labs still strongly relies on traditional microbiological techniques. However, over the past years, molecular detection techniques have increasingly become popular, allowing faster and more sensitive detection. Although these techniques are relatively easy to operate, many requirements must be met to ensure reproducibility and reliability of molecular methods. The session provided insight in requirements for qualitative and quantitative PCR methods to contribute to ensuring molecular test reproducibility and quality. Chaired by Tetsuhisa Goto of Central Scientific Commerce, Inc. and Scott Leppanen of Agilent Technologies, speakers introduced new ISO standards related to PCR and real-time PCR quality control.
In “Ensuring the Reproducibility and Quality of Quantitative PCR–The Role of MIQE Guideline,” Leppanen outlined the process of performing real-time qPCR, including sample handling, extraction of nucleic acid and its quality, reverse transcription, PCR, and analysis and visualization of raw qPCR data. He also focused on the role of the “Minimum Information for Publication of Quantitative Real-Time PCR Experiments” (MIQE) guidelines in providing guidance on information that should be reported as part of an experiment to ensure proper interpretation and reproducibility of data, and conclusions drawn from them.
To ensure quality and accuracy in genetic testing, ISO 20395 “Biotechnology–Requirements for Evaluating the Performance of Quantification Methods for Nucleic Acid Target Sequences–qPCR and dPCR” provides useful information regarding design of procedure, sample quality, optimization of the methods, validation, traceability, and measurement uncertainty. This standard is helpful not only for establishing accurate measurement methods but also for evaluation of a working standard in the laboratories, says Hiroki Nakae of Bio Business Solution Co. Ltd.
To provide quality assurance of PCR assays through thermal cycler calibration and method validation, the revised ISO 20836 Standard describes a universal performance testing method for thermal cyclers, used for DNA-based food safety testing. The revised ISO Standard has been elaborated with an integrated approach in which thermal cycler variation is taken into account during method validation in order to assure the quality of the test results. “We carry a huge responsibility in food testing, and we hope to contribute to reliable testing,” says speakers Mary Span of Cyclertest; Marc Verblakt of CelciusLabs; and Tom Hendrikx of Cyclertest.
In Standardization of DNA-Based Methods for Food Testing, speakers Masunori Kajikawa, Yuki Yonekawa, and Satoshi Nakazawa of RICOH Company Ltd.; Ian Ryztyan Kajikawa of FASMAC Company Ltd.; and Kazumi Kitta of National Agriculture and Food Research Organization provided an overview of ISO 20813:2019, which specifies minimum requirements of performance characteristics for detection, identification, and quantification of nucleic acid sequences (DNA) from animal species by molecular biological methods. In addition, speakers introduced an evaluation method for detection and quantification limits in quantitative analysis using newly developed standard materials with the number specified in a single copy unit. Accuracy is a key performance indicator for testing to keep foods safe.
FDA’s Sensory Methodology and Sensory Analyst Training and Qualification
The federal Food, Drug and Cosmetic Act defines foods as adulterated if they consist in whole or in part of any “filthy, putrid, or decomposed substance.”
This session, presented by Benjamin Phillips and Heather Hawk of the U.S. Food and Drug Administration, introduced sensory analysis of seafood and the FDA’s Seafood Sensory Program’s SOP which describes a protocol for sensory analysis of seafood using color, texture, and odor. FDA has also developed a system to qualify seafood sensory analysts. Using samples that have gone through controlled decomposition, analysts are trained and their performance determined to be qualified up to various levels.
Seafood Decomposition: Bacterial Communities Associated with Chemical and Sensory Tests for Decomposition
Can chemical analysis complement or replace traditional history- and sensory-based analysis of seafood decomposition? Kristin Butler of the U.S. Food and Drug Administration introduced research examining the relationship between bacterial communities and chemical/sensory attributes produced during spoilage. This will help determine how recent advances in next-generation sequencing (NGS) can make culture-independent analysis of bacterial communities possible. Next steps include research on correlation of chemical analysis to sensory techniques and other parameters.
Determination of Decomposition in Fishery Products by Mass Spectrometry with Sensory-Driven Multivariate Analysis
Randy Self of the U.S. Food and Drug Administration described a project to compare sensory and analytical techniques using a large sample set from 23 seafood products subjected to controlled decomposition to produce seven discrete quality increments. Each sample was analyzed first by sensory analysis, then extracted and analyzed using LCMS. Using “random forest” data analysis, they created a model for predicting what the sensory score might be based on certain compounds, and compared this with actual sensory scores. The finding of decomposition state of each sample was consistent with sensory for 99.6% of samples (n=550).
Analysis of Biogenic Amines by LC-MS/MS
Sarah King of Eurofins Central Analytical Laboratory presented on biogenic amines, a class of low molecular weight amines produced during metabolic decomposition that have toxicological effects. There is a wide array of methods for determining biogenic amines by monitoring the presence of histamine, putrescine, cadaverine, and tyramine, or lack of spermine and spermidine. However, these methods lack specificity and have high limits of quantification. In their research, they validated as accurate and precise a LC-MS/MS method on a tuna matrix. The method is applicable to fish and fishmeal based on sensory comparison and proficiency testing.
Simultaneous Determination of Six Underivatized Biogenic Amines in Canned Tuna by LC-MS/MS
Sensory analysis for seafood requires unique and highly specialized skill sets with extensive and rigorous training, while the ELISA assay is slow and not sensitive, and the HPLC method with fluorometric detection is laborious and requires a derivatization step. In this presentation, Eugene Chang of the U.S. Food and Drug Administration described the development and validation of an efficient method for detecting 6 biogenic amines in canned tuna using LC-MS/MS without derivitization. The extraction method requires just two steps.
Hi, this is Marida, continuing our coverage of the Annual Meeting. Unfortunately, our bloggers were unable to cover two sessions at once this morning so I have summarized this session’s advance information for you below.
Internationally, with the consumer demand for “natural” colors increasing, some food manufacturers are turning away from synthetic color additives and towards those from plant extracts or other natural sources. Under current US regulation, color additives fall into two categories: those subject to FDA’s certification process which include synthetic color additives and are tested by the FDA, and those that are exempt from certification where it is up to manufacturers to comply with specifications. From a quality and safety perspective, for colors from natural sources, there is a general lack of product definitions or publicly available purity, quality, and safety specifications that are consistently applied. Consistent industry-wide safety standards are needed and methods for microbiological contamination, heavy metals, pesticides, and unauthorized solvents can help establish these standards. This Scientific Session covered key potential safety hazards affecting sourcing and analytical science challenges to continue the conversation on next steps for our AOAC Community on Color Additives.
Validation Guidelines for On-site PCR Based Botanical Species Identity Testing to Support Quality Control of Botanical Dietary Supplements
Steven Newmaster of the University of Guelph discussed his research on gaps in PCR-based molecular diagnostic tools, the most commonly used DNA-based identity tool, routinely used to identify foodborne pathogens and allergens in food. After a survey of the literature indicated that some validation criteria are not addressed when developing PCR tests for botanicals, he showed how properly validated PCR methods can be developed on small, real-time biotechnology that can be placed directly into the supply chain ledger in support of highly transparent data systems that supports quality control from farm to the fork of the consumer.
Portable Real-Time PCR Instrument for Botanical Raw Materials Identification in the Field
Stefano Lo Priore of Hyris Ltd discussed how genetic data provide valuable information in the assessment of raw material and process quality in industries that use natural products as base ingredients. So far, lack of laboratory infrastructure and logistical challenges have prevented widespread implementation. He discussed a mobile genetic analysis solution that can be adopted in a manufacturing environment, integrating real-time continuous data collection with standard SPC quality control strategies for novel insights into natural products incoming quality control.
Industrial and Field Authentication of Herbal Material Using DNA Barcoding
Jiang Xu of the China Academy of Chinese Medical Sciences introduced a pipeline for rapid, accurate, and specific authentication of certain species without using electric equipment. Using the example of Gelsemium elegans, a poisonous flowering plant that is widely distributed in southern China and Southeast Asia, he demonstrated the efficacity of a method combining fast DNA extraction and RPA for portability and usability in the field to profide onsite identification of species, including herbal and animal materials, whether toxic or not.
Extending Botanical Identification from Laboratory to Farm: Industry Experiences on Authentication of Botanical Materials in the Field
Zhengfei Lu of Herbalife Nutrition, working with colleagues from Herbalife Nutrition, Agilent Technologies, and Mars Global Food Safety Center, attacked the issue of correctly identifying and sourcing botanicals. While the current model requires off-site quality evaluation, this is slow and field identification can save money. He showed a video illustrating the effectiveness of portable molecular analytical devices, using the example of identifying German chamomile on the farm. Results aligned with those from laboratory equipment. “This fit for purpose test can be used in diverse settings as a good complement to laboratory analysis,” he concluded, ” A portable device based field testing has the potential to be a fast, reliable, and effective tool in the first line of defense of botanical quality control.”
In the closing presentation of the Wiley Award Symposium, George Joseph of AsureQuality discussed Gaps in Harmonization of Expression of Vitamins Content in Food and Dairy Products.
Food supply and consumption around the world are becoming ever more interconnected, and along with it are human and farm animal health and the global environment.
The analytical methods in use do not have a harmonized approach on how the quantified amounts of vitamins and their vitamers should be expressed for labeling purposes for global market. There is a real lack of information on how the vitamins and their vitamers can be converted in relevant (international) units and/or activity. This can lead to difference between the analytical results of different laboratories and consequently to a misunderstanding of the results expressed in vitamin content and in some cases in vitamin activity on the product label.
“Honey is not just for spreading on toast,” is how Megan Grainger of the University of Waikato started out her presentation on the antibacterial properties of honey.
Honey has three main antibacterial properties that slow or prevent growth of bacterial species. Honey is used for wound dressings to keep wounds moist but also because it is non-toxic, reduces scarring, and bacteria cannot develop resistence.
Dr. Grainger illustrated this benefit with a progression of images (“Not too gory!” she promised) demonstrating the effectiveness of honey in healing a leg wound that had not responded to other treatments for bacterial infection.
In her presentation, Conversion of Dihydroxyacetone to Methylglyoxal in Aotearoa Mānuka Honey: Forecasting the Unique Non-Peroxide Antibacterial Activity, she discussed the unique properties of Mānuka honey, which comes from bees collecting nectar from the Mānuka tree flower and has non-peroxide antibacterial activity not found in other honeys. It contains high quantities of Methylglyoxal (MGO), the compound responsible for this activity. Recently, this honey has been selling for high prices and New Zealand’s Mānuka honey exports were worth NZD$325 million dollars in 2019.
Dr. Grainger’s presentation detailed her successful research to develop a forecast model for the conversion of DHA to MGO to find optimum parameters for storage.
This is Marida, back keeping you updated on today’s events.
The symposium kicked off with an overview by Steve Holroyd of Fonterra Co-operative Group, on Infrared Spectroscopy for Dairy Analysis in Aotearoa. Aotearoa, literally translated as “land of the long white cloud,” is the Maori name for New Zealand.
Holroyd noted that infrared spectroscopy has been used routinely to quantify the composition of milk and milk products for over 30 years, and developments in hardware, software and analytical statistics have widened the scope of application to include the entire range of dairy products throughout the production chain. Challenges such as sampling, sample preparation, instrument networking and the development of generic calibrations have been met and overcome, making infrared spectroscopy an indispensable component of dairy processing safety and quality today.
This was followed in the Symposium by Brendon Gill of Fonterra presenting on Analysis of α-Tocopherol Stereoisomers in Infant Formula by Chiral Chromatography. Measurement of the biologically active α-tocopherol content in infant formula presents a significant analytical challenge, requiring chiral separation of the α-tocopherol stereoisomers.
Hi, this is Tien, taking over the blog for the Wiley Award Address.
As they near the end of their productive careers, Wiley Award winners Harvey Indyk and David Woollard reflected on more than 40 years of contributions from New Zealand scientists to AOAC and the analytical communities, specifically the dairy industry. Since Indyk’s and Woollard’s early careers, vitamin analysis was an important part of their activities, starting with vitamin A in dairy products. This led to routine determination of vitamin A esters in milk powders, followed by concurrent detection of vitamin E acetate in infant formulations. The duo was the first to report natural fluorescence of tocopheryl acetate, among many other notable accomplishments.
Over the years, analytical techniques in food composition have evolved tremendously. Another significant change is evolution into what is known as “big data” era. But despite these modernizations, one thing will always remain the same and that’s the need for reliable methods, said the joint winners.
They hope that the next generation of New Zealand scientists will continue efforts to assist AOAC in its mission of providing validated chemical and microbiological methods across many sectors, promote New Zealand analytical science, and grow professionally and personally.
2020 Awards Ceremony
AOAC President Henry Chin and Executive Director David Schmidt teamed up again to recognize the contributions of leaders in the AOAC’s analytical science community. Immediately after the announcement, AOAC issued an announcement on the winners.
Keynote Address presented by Gilles Martin of Eurofins Scientific
“A lot has happened in my 33 years in the field,” commented Dr. Martin in the Q&A session following his address, “But what has not changed is that methods still need to be reliable.” He noted that what was once the focus of a few people has now become the accepted norm.
He used the example of the covid pandemic: “There is already a lot of work to do to validate all those methods, to make sure the sensitivity of those methods can be compared.”
On the technology side, when he started with testing pesticides, he said they could test for 50 analytes, and that could require multiple methods. “Today we can test for 400 methods, sometimes more, in one run.” The technology is becoming more powerful; the software tools that are available to make use of data have evolved dramatically. Now we can measure the whole genome for less than $1000…and miniaturization will put these tools on bench tops and even in doctor’s offices. “But one thing that will not change is the need to make sure these tools are reliable, especially as we move to point of care more and more.”
The live Q&A followed his Keynote Presentation, The Potential of Testing to Protect our Environment and the Health of All. “There has never been a better time for innovation in testing,” he said, noting that:
– instruments are getting more sensitive and cheaper;
– computers and artificial intelligence tools are breaking new frontiers in data storage capacity, speed and power;
– the internet is allowing scientists globally to access and exchange data in real time; and
– thanks to AOAC and other standards bodies, a culture of validated reliability for testing is emerging.
He concluded with a message for young scientists: “For young scientists who today want to decide where to go, the testing field, the analytical sciences will offer enormous possibilities.”
2020 Welcome and announcements
Kicking off the second week of the AOAC Virtual Meeting, AOAC President Henry Chin and Executive Director appeared side by side in a conversational virtual welcome and “status check” chat. They presented an overview of AOAC’s accomplishments and new initiatives since the last Annual Meeting. Both thanked the many volunteers who make it all happen, and Dr. Chin called out the special contributions of the current Board of Directors. He then announced the names of the incoming board members:
– Erin Crowley – President
– Henry Chin – Past President
– Anthony Lupo – President Elect
– Mary Kay Krogull – Treasurer
– John Szpylka – Secretary
– Nuri Gras Rebolledo – Director
– Danièle Sohier – Director
– Stephen Wise – Director
– Clay Detlefsen – Director
– Samuel Godefroy – Director
– Bert Popping – Director
Retiring from the Board:
– Brad Goskowicz, who hasserved as Director, President Elect, Pres, and Past President (2013-2020)
– Lei Bao, who has served two terms as Director (2014-2020)
Hi, this is Tien, taking over the blog for one last post on the Annual Meeting’s first week.
AOAC just wrapped up its first week of the Virtual Annual Meeting with the Cannabis Analytical Science Program (CASP) meeting filled with exciting activities much needed by the community. AOAC CASP working groups have developed draft laboratory guidance for drying field-fresh hemp plant samples and Standard Method Performance Requirements (SMPRs) for a screening method for mycotoxin contaminants in cannabis plant material and cannabis derivatives (SMPR for quantitative method to come) and for Shiga toxin-producing Escherichia coli (STEC) in cannabis and cannabis products. Be sure to make your voice heard and comment and vote on these standards.
CASP working groups have also been busy developing recommendations for training and education to bridge knowledge gaps and for technical requirements needed to develop a proficiency testing program for cannabis and hemp.
CASP is also in the works for joint collaboration with the Hemp and Cannabinoid Science Institute to recognize and promote each other’s work related to analysis of hemp and cannabis.
Future work will have a more product-centric focus (for example, gummies), which will offer more consistency and uniformity across working groups, says CASP Program Lead Scott Coates. Also stay tuned as CASP launches an Emergency Response Validation (ERV) Program for yeast and mold in cannabis flower.
Coates said he is very happy; this is exactly what he hoped for when AOAC set up CASP two years ago. “I envisioned it as a mini-AOAC, with all the parts that AOAC has, but just focused on cannabis. Now with the addition of the working groups for Proficiency Testing and for Training & Education, we’re pretty much where I had hoped we would be. It is much needed by the community.”
Chair Walter Brent Wilson is reporting out on the new CASP Proficiency Testing Working Group, another crying need in the cannabis industry.
The group is designing a comprehensive Proficiency Testing program for cannabis and hemp. Current subgroups include the cannabinoids, moisture, terpenes, heavy metals pesticides, and mycotoxins; future work will include microbials and residual solvents.
This presentation should be of interest to cannabis labs and scientists across the country and around the world.
Dr. Toby Astill has been the driving force behind the new CASP Training and Education Working Group and as Chair, he has taken it from an idea to a reality. The group has representatives over 60 organizations BUT – they need more experts to fill out the panels and he urged people to reach out to him if interested.
Toby and his group started with a survey of what topics the cannabis community is interested in, ranging from the history of cannabis and hemp to clinical research concepts and how to navigate the state/federal legal landscape. They’ve also decided that distance learning is going to be a big part of training, unsurprisingly in the current Covid situation.
The group has settled on starting with a 4-part webinar series, starting with microbial testing and heavy metals and continuing with pesticide or mycotoxin analysis and setting up a lab/regulatory.
“We need to work on this together – if you’ve got energy or experience, think about joining!” Reach out to him at [email protected]
Julia Bramante, who is Chair of the CASP Microbial Contaminants Working Group, has just finished reviewing the status of SMPR development in the group. They’ve got one SMPR completed for shiga toxin-producing E. coli in cannabis; the public comment period has ended and it’s out for an eBallot. The next step is publication in the AOAC Official Methods of AnalysisSM.
Julie Kowalski, Chair of the CASP Chemical Contaminants Working Group. She shared a slide with the impressive number of organizations represented on the Working Group. Her talk is focused on her group’s activities developing an SMPR for screening for mycotoxins. The SMPR is currently in eBallot, and the next step will be publication in the AOAC Official Methods of AnalysisSM.
Here’s the Q&A:
Q: Would it be acceptable to submit a method for total aflatoxin, ochratoxin and zearelenone?
A: Yes – the SMPRs are the minimum requirements. If you have additional toxins you want to add, that should not be an issue. That would be great!
Dr. Holly Johnson, Chair of the CASP Cannabinoids and Consumables Working Group, is reviewing the group’s activities over the past year.
For the last six months her working group has been developing guidance on the dry-weight aspect of testing, greatly needed by labs that are required to test materials that are delivered to the testing lab in field-fresh condition, but must then dry the material – a crucial step but one that is not well defined.
Dr. Johnson is now taking questions:
Q: Do you see any potential ‘glitches’ that a lab may encounter?
A: The biggest glitch is to keep in mind what the fit for purpose aspect is for this step.
The Cannabis Analytical Science Program meeting has started. The agenda looks amazing – we’ll be hearing from Dr. Ethan Russo, Founder of CReDO Science, Dr. Holly Johnson of the American Herbal Products Association, Dr. Julie Kowalski, Consultant, Julia Bramante of the Colorado Department of Public Health & Environment, Dr. Toby Astill of PerkinElmer, and Dr. Brent Wilson, NIST. What a line up!
“Cannabis Chemistry Potpourri” – In this fascinating talk, we’re getting a detailed review from Dr. Russo of the many and varied compounds in cannabis, where they are found in the plant and their medicinal properties. Among others: anti-anxiety, antidepressant, analgesic, cancer cytotoxic agent, weight loss, anticonvulsant.
Selective breeding can be very effective in tweaking the combination and relative proportions of compounds, to treat specific conditions, such as epilepsy.
On a more negative note, contamination from pesticides is sobering, with one study showing 24 insecticides in legal cannabis tested from Washington State.
Dr. Russo had time to answer just some of the many questions submitted. Here are some:
Q: What are the main analytical challenges?
A: There is a profusion of labs, people think they can take a quick course, set up a lab, and make a million dollars. But this stuff is difficult! You’re dealing with lipophilic substances that stick to everything; cannabinoid analysis is not simple and terpenoids is even harder.
Q: If you were putting your money on one minor cannabinoid to take into the clinic which would it be?
A: That’s easy: cannabigerol is the next big thing. It has tremendous potential and should be included in any cannabis extraction for its antianxiety activity with no sedation, its anti cancer and antibiotic effects.
The Glycerol Esters of Wood Rosin Working Group meeting got down to business with an overview of work to date presented by AOAC Technical Consultant Sharon Brunell.
Glycerol esters of wood rosin are compounds derived from pine tree wood through solvent extraction and steam distillation, and are used in products like chewing gum and for adjusting density of citrus oils in beverages. The Working Group has developed an SMPR for characterization and quantitation of component fractions, residual resin acids, monoesters, and neutrals. It is currently out for public comment.
A more in-depth look at the SMPR was presented by Giorgia Purcaro, Chair of the Working Group.
5:00pm-6:30pm (Sponsored by Abbott)
Marida’s update: Having fun at the Virtual Welcome Reception!
This is Tien from AOAC, and I am taking over the blog for the remainder of this session. Here’s my update:
– There will be an overview of draft SMPRs but voting will not be live. There will be an E-ballot after meeting.
– We are not voting on all SMPRs as some SMPRs are just in the launching stage like chlorate/perchlorate.
-AOAC SPIFAN is launching a working group to develop SMPRs for quantitative determination of chlorate and perchlorate in baby foods and infant formula ingredients and finished products. Interested in joining this work group contact AOAC.
Melissa Phillips of NIST has completed an update on NIST reference materials and we are moving on to a presentation by Don Gilliland of Abbott on the AOAC Infant Formula Advisory Task Force. Initially, the Task Force was formed to develop a proficiency testing program for infant formula, leveraging AOAC’s PT program. It is now focusing on an Education/Quality Program to improve laboratory expertise and identify challenges, with a goal of improving laboratory practices.
The Working Group meeting is being chaired by Darryl Sullivan, Eurofins Food Integrity and Innovation. He’s reviewed AOAC antitrust and volunteer policies, and the meeting is on.
It kicked off with a report out from Erik Konings of Nestle reviewing the AOAC China Section including Vitamins A&E Comparison & GB Pilot Study. As part of updates on Codex, Sullivan and Dustin Starkey of Abbott are discussing Sweetness. “Sweetness is a complex, subjective concept based on sensory perception; verifying verifying regulatory compliance would be incredibly difficult.”
Sullivan noted that the group would welcome new subject matter experts, especially carbohydrate experts and people with knowledge of sensory experience.
Deborah McKenzie has given an overview on the SMPR process and now is summing up the work to date by this Working Group, and touching on next steps. “This working group has quite a bit to accomplish.”
McKenzie is summing up after emphasizing that AOAC would welcome new members to the Molecular Applications, Targeted and Non-Targeted testing Working Groups for botanicals and spices. She concluded with a link to sign up.
We have a provisional result from priorities poll:
1. Turmeric / Vanilla (tied)
2. Spices (group)
We’re now in the discussion.
After a break, we are now into the working session of the Botanicals and Spices Working Group meeting. This group has focused on olive oil, honey and milk and we heard a report out starting with Non-Targeted Testing. John Szpylka of FSNS reviewed technologies for NTT SMPR development. “The definition of food fraud: A deliberate act to increase the apparent value of an ingredient or finished products this is reference to economically motivated adulteration.”
Joe Boison of EJ Consultancy reporting out on Targeted Testing, who noted that fraud may pose a health risk to consumers, even though it is economically motivated, such as the case with nut protein in cumin and paprika. Rapid Screening Techniques are required to detect and help prevent fraud from occurring in the industry. He discussed the need for gap analysis for the adulterants in Botanicals and spices.
This was followed by an update from Daniele Sohier of ThermoFisher on technologies for SMPR development for Molecular Applications as it pertains to botanicals & spices.
The Food Authenticity Methods Working Group meeting has started with an introduction to the topic by Bert Popping of FOCOS, who discussed stakeholder interactions and transparency of the process along with how the current processes are being utilized to address the needs for botanicals and spices.
Stakeholders are now being asked to go to a form to vote for their top three botanicals and spices for prioritization among:
– Aloe Vera
– Natural flavorings
– Spices (group)
The meeting continued with global perspectives on botanicals and spices, starting with a presentation by the European Spice Association’s Jean-Louis LaFeuille (McCormick) and Greg Corbishley (Bart-Ingredients) who discussed analytical issues, including those currently high risk for adulteration.
Moving on to botanicals, Sibyl Swift (Natural Products Association) gave a presentation on botanicals including those currently high risk for adulteration.
Morning session: 9:00am-10:45am (rescheduled from Wednesday)
What are the future analytical challenges for effective enforcement of EU food safety legislation? Analytical tools must give reliable reproducible results, quickly, and at a reasonable cost. Dr. Frans Verstraete, Ph.D., Deputy Director General for Food Safety at the European Commission Health And Consumers Directorate-General, is giving some concrete examples on how this plays out on the ground.
The “Methods cascade” in the EU means methods must comply with EU performance criteria or some accepted alternatives. But we sometimes lack a robust method altogether even as we see many new areas for regulation, such as micro- and nano-plastics, PFAS, brominated flame retardants, methyl mercury, quinolizidine alkaloids, and furans.
One market – One standards: Overview of ARSO within the Africa Continental Free Trade Area
“Information is key,” says Dr Hermogène Nsengimana, Ph.D, Secretary General of the African Organisation for Standardisation (ARSO), about the Africa Trade Web portal.
He is describing how ARSO works within the AfCFTA to build a quality infrastructure in Africa. Kenya, Egypt, and South Africa are doing well but there is work to be done to build capacity in most other countries.
Looking at challenges in harmonization of standards and technical regulations, he is illustrating realities on the ground with a gap analysis of the large and important cassava sector in African top producing and consuming countries.
The standards developed in different member countries for cassava and cassava products vary widely, from the number of parameters specified to the limits of requirements for key parameters such as moisture content, heavy metals contaminants and pesticide residues. “We have very few standards for cassava in general, and test methods are absent or disparate,” he notes. “We cannot harmonize if we cannot agree on test methods.” This highlights the need not only to harmonize standards but to develop simultaneously common testing methods, for this unique African product and across the board.
Supporting Improvement of the Quality of Testing in Africa
In the first Plenary presentation of the Analytical Solutions Forum, we’re hearing some fascinating details on how AOAC is building food safety capacity in Africa. Dr. Owen Fraser, President of the AOAC Sub-Saharan Africa Section, says Africa is at a food safety crossroads. Rapidly rising population, the formation of the Africa Continental Free Trade Area, and increased international trade both in Africa and around the world, the need for food safety infrastruction has grown. Since 2018, when the Section was formed, it has promoted best analytical science practices in the region using collaboration, training and education, methods development and harmonization to establish itself as an independent and impartial scientific advisory body.
Afternoon session: 2:00pm-4:30pm
We’ve just been told that due to the internet outage this morning that affected our Virtual Annual Meeting platform, the three Analytical Solutions Forum Plenary Session presentations listed below have been rescheduled to tomorrow morning, September 10 from 9:00am – 10:45am ET.
– Supporting Improvement of the Quality of Testing in Africa
Dr. Owen Fraser, Ph.D., President, AOAC Sub-Saharan Africa Section
– One market – One standard: Overview of ARSO within the AfCFTA
Dr Hermogène Nsengimana, Secretary General, African Organisation for Standardisation (ARSO)
– Future analytical challenges for an effective enforcement of EU food safety legislation. The example of contaminants in food.
Dr. Frans Verstraete, Ph.D., Deputy Director General for Food Safety, Directorate General Health and Food Safety, European Commission Health And Consumers Directorate-General
Tools to combat food fraud
Dr. Franz Ulberth, Head of the Fraud Detection and Prevention Unit at the European Commission’s Joint Research Centre, has just rounded out this session’s topic with a description of the complex legal and institutional framework in the EU dealing with food fraud, and how a recent stock-taking exercise flagged early warning systems, compositional databases of vulnerable foods, and the creation of centres of competence as priorities.
Early Warning Signaling in Food Safety
Can we flag food safety risk hazards before they hit the supply chain?
Regulatory bodies early warning systems like the World Health Organization’s International Food Safety Authorities Network (INFOSAN) and CORE (US FDA) are collecting and maintaining databases of information on potential hazards; and the private sector is also producing early warning signaling systems. The combination of collective knowledge, artificial intelligence, and an open global network offers horizon scanning intelligence that complements traditional HACCP, facilitates public – private partnerships, and moves food safety into the 21st century.
Dr. Peter Embarek of the World Health Organization’s INFOSAN Secretariat is discussing early detection and management of food safety events at the international level, and how new technologies will shape food safety management in the future.
INFOSAN is the international mechanism used by national food safety authorities to share information on international food safety events to minimize impact.
He is illustrating how with examples like the outbreak of Listeriosis linked to internationally distributed frozen vegetables from Hungary, where complex global distribution patterns and the nature of the product made this the largest event INFOSAN has ever dealt with. INFOSAN hopes to become a “network of networks” that facilitates information sharing.
Chemometric and Artificial Intelligence Applications to Control Risk in Food Safety
We have data, data, and more data. Sophisticated analytical methods turn out terabytes of data in a single analysis, but all this data is meaningless without context and interpretation.
Dr. James Harnly, Ph.D. of the U.S. Department of Agriculture just spoke on work being done at the newly organized Methods and Applications Food Composition Lab. He is responsible for Food Data Central, the new USDA food composition database and its analytical support group.
In this second day of the Emerging Topics and Technologies session, he is presenting some examples of deconvolution of data using chemometrics with machine learning to convert vast amounts of raw data into information and knowledge using machine learning.
He concluded that detection of patterns remains the ultimate goal – and deconvolution of experimental factors is essential to this and allows determination of the statistical significance of each factor.
Morning session: 9:00am – 12:00pm
Perspectives from the Analytical Steering Committee: An Open Discussion, cont.
The open discussion had just started when the virtual platform developed technical issues. Waiting for the feed to come back online.
Perspectives from the Analytical Steering Committee: An Open Discussion, cont.
“AOAC is now more proactive than it has ever been in any time in its rich history, so this is the time to get involved,” says Darryl Sullivan of Eurofins.
Perspectives from the Analytical Steering Committee: An Open Discussion
ASF Day Two is off and running with an overview from members of the Analytical Steering Committee, an advisory body representing AOAC stakeholders. They are tasked with identifying new AOAC initiatives with the highest stakeholder interest, analytical science need and potential public health impact.
Committee Chair Melissa Phillips of the National Institute of Standards & Technology has kicked off the discussion with biographical introductions from the Steering Committee members:
– Morgan Wallace, Rheonix, Inc.
– Darryl Sullivan, Eurofins
– Erik Konings, Nestle
– Cheryl Lassitter, NOAA
– Hong You, Eurofins
– Brooke Roman, Neogen
– Aniko Solyom, GAAS Corporation
– Pat Bird, PMB BioTek Consulting
– Jin Tan, Abbot Nutrition
– Selen Stromgen, FDA
– William Shaw, USDA
– Solomon Kariuki, Univ. of Kentucky
Afternoon session: 2:00pm-4:30pm
In silico Analysis, cont.
AOAC’s Chief Science Officer, Palmer Orlandi has just urged everyone to stay tuned: A new AOAC proposal is coming shortly that will go beyond the SPADA in silico work, and use what was developed in the last part of that program to move forward in the world of genomic sequencing, bioinformatics, and more.
His comments followed a presentation by AOAC Consultant Dr. Sharon Brunelle on in silico analysis where she gave an overview of the AOAC Research Institute’s Emergency Response Validation for Detection of SARS-CoV2 on Surfaces.
Laboratory determination of inclusivity and exclusivity is time-consuming, expensive, and is usually limited to at most 150 species/strains. In silico analysis has a significant advantage over wet-lab testing alone in that genetic sequences from tens of thousands of target strains and near neighbors can be analyzed for inclusivity and exclusivity.
“Imagine the advantage of testing 15,000 versions of organisms rather than hundreds,” commented Scott Coates, Director of the Research Institute.
Dr. Brunelle wrapped up her presentation with a status check: With eight method developers participating, the SARS-CoV2 Emergency Response Validation project now has completed in silico reviews and is moving on to the independent laboratory matrix study phase. The expectation is that certifications will be awarded in October.
In silico Analysis, cont.
Why do we need a standard for in silico analysis in assay development? Cost, time and effort, says Dr. Shanmuga Sozhamannan, Technical Coordinator for the Defense Biological Product Assurance Office within JPEO JPL CBRND Enabling Biotechnologies.
He is discussing the roles for in silico approaches in molecular assay design including recent advances in Whole Genome Sequencing technologies, with the goal of minimizing expensive and time consuming experimental work by taking advantage of the sequence databases and doing thorough bioinformatics analysis. “We need a more modern paradigm using in silico approaches.”
In silico Analysis
Kicking off the last session of today’s Analytical Solutions Forum, John SantaLucia, Jr., Ph.D.,(Professor, Wayne State University and CEO, DNA Software, Inc.), is discussing recommendations for developing molecular assays for microbial pathogen detection using modern in silico approaches. He discussed how in silico approaches can improve molecular assay development process and reduce the time and cost by utilizing available databases of whole genome pathogen sequences combined with modern bioinformatics and physical modeling tools.
PFAS: The “Forever” Chemicals
Dr. Susan Genauldi, a Research Chemist in the Center for Food Safety and Applied Nutrition at the Food and Drug Administration, is answering questions from the audience on the FDA’s a long history of investigating per- and poly-fluoroalkyl substances in food and food packaging after an overview of research on PFAS.
Previously, we heard from Dr. Neal Saab, Senior Program Manager at ILSI North America where he leads scientific committees focused on food, chemical and packaging safety. ILSE NA recently held a symposium on science gaps in risk assessment of PFAS in food. Dr. Saab summarized key findings and proposed approaches to address the science gaps in risk assessment of PFAS in food.
This session generated a high volume of questions from the audience, such as:
– Are PFAS GRAS? Also, which chemical companies manufacture PFAS?
– Since contamination of ground water by PFAS, would bottled be tested by FDA?
– Does the total dietary study take into consideration intake from dietary supplements and herbal products?
Morning session: 9:00am – 12:00pm
Plenary Presentations, cont.
In the second plenary session, Dr. Kaushik Banerjee, Chairman of the AOAC India Section, just finished his presentation on”Food safety framework of India and implementation of AOAC standards for analytical capacity building.”
In addition to working closely with the Food Safety and Standards Authority of India (FSSAI) to foster the strategic responses to food safety regulations, the section is advancing capacity building, expanding and developing methods that are fit for India’s unique food matrices, and mentoring young analytical scientists through their annual meeting’s Young Scientist Award and Woman in Analytical Science Award.
The first plenary presentation has started, with Dr. Nuri Gras Rebolledo, Ph.D., Executive Secretary of The Chilean Food Safety and Quality Agency. She is discussing food safety and food supply chain challenges from a Latin American perspective, from food security to food sustainability and food safety, including Covid 19.
She noted the World Health Organization’s recent report on the global burden of foodborne diseases reaches 600 million cases, or 1 in 10 people, with an estimated 420,000 deaths worldwide.
She is highlighting that capacity building is a real need in low and medium income countries. “We need to work together in a transparent way, in a multidisciplinary approach that includes government, academia, the private sector, and society in general.”
Answering questions from the audience, Dr. Rebolledo noted that the Covid-19 pandemic may have a silver lining for the future of analytical science in Latin America. “I think that young students have not found analytical chemistry that attractive in recent years, but Covid-19 has raised their awareness of the importance of science. This is a big opportunity for the younger generation.”
This is Marida from AOAC, and I will be updating you on the Annual Meeting, with some help from other AOAC colleagues.
Updates on AOAC INTERNATIONAL’s Core Science Programs
The Annual Meeting has started! Palmer Orlandi, AOAC Chief Science Officer and Deputy Executive Director, kicked off the 2020 gathering with welcome and introductory remarks in the start of the morning session of the Analytical Solutions Forum.
So far we’ve heard updates from Scott Coates, Sr. Director of the AOAC Research Institute and from Arlene Fox, Sr. Director of AOAC’s Laboratory Proficiency Testing Program. These were followed by a thorough update on AOAC’s core science programs from Deborah McKenzie, Sr. Director of Standards at AOAC. She just noted that in AOAC’s new role as US TAG to ISO/TC 34 (Food products), AOAC has been successfully working to increase industry participation.
AOAC INTERNATIONAL brings together government, industry, and academia to establish standard methods of analysis that ensure the safety and integrity of foods and other products that impact public health around the world.
2275 Research Blvd, Ste 300
Rockville, MD 20850
+1 (800) 379-2622