Important Considerations for Developing Reliable Methods for the Analysis of Chemical Residues in Foods (Food Safety)

Why Should You Attend:

Food Safety, regarding chemical contaminants in food is a growing field of analytical chemistry. With the availability of sensitive and selective instrumentation such as mass spectrometry, proper use of sample preparation is often overlooked. For example, since the pesticides registered over the last decade are mostly polar compounds that are not amenable to gas chromatographic techniques, LC-MS/MS is the methodology of choice to monitor these contaminants in foods for enforcement purposes. Likewise, LC-MS/MS is needed for the reliable determination of other polar food contaminants such as mycotoxins, veterinary drugs, and melamine and its analogs.

Although LC-MS/MS offers several advantages in terms of sensitivity, selectivity and overall speed of analysis, there are several important considerations which must be kept in mind when developing analytical methods that rely on this technology. Some of these critical components include: extractability; test portion cleanup; specific chemical properties of analyte such as polarity and pH of analyte; choice of internal standards and how to properly use them; spiking of test portion versus incurred residue analysis; ruggedness; proper identification and the use of standard reference materials (if available) and/or proficiency test samples. The impact of these critical components on method development will be discussed using well known examples of challenging problems such as the analysis of over 200 polar pesticides in foods and dietary supplements, mycotoxin analysis, food adulterants, plus other examples of current interest.

Learning Objectives:

• Ways to compensate for matrix effects to ensure accurate quantitation of chemical residues in food
• How to decide between using low-resolution or high-resolution mass spectrometry
• Best practices for spiking of test portion versus incurred residue analysis
• The proper use of standard reference materials and proficiency test samples
• Proper ways to identify compounds to avoid reporting false positives or false negatives that can lead to embarrassing situations for the laboratory
• Efficient methods for sample preparation
• QuEChERS (Quick, Easy, Cheap, Effective, Reliable, Safe) for Sample Preparation
• Examples will include: Pesticide Analysis, veterinary drugs, mycotoxins, botanical dietary supplements, analysis of active pharmaceutical ingredients in dietary supplements

Who Will Benefit:

Staff in food analysis laboratories at government laboratories, food industry laboratories, contract research organizations, and others including:

• Anyone analyzing food or developing analytical methods for food analysis, particularly in chemical residues analysis
• Staff in food analysis laboratories at government laboratories, food industry laboratories, contract research organizations, and others

Alex Krynitsky
Director, Symbiotic Research LLC

Alexander (Alex) J. Krynitsky currently assumes a wide range of business development, scientific, and technical duties associated with various animal, aquatic, plants, and soil environmental fate and metabolism projects performed at Symbiotic Research. He also mentors’ younger scientists in separation science techniques (LC–MS, CE-MS, and GC–MS), and in sample preparation. Alex is very active in the AOAC International and has been a section editor for J. AOAC International for residues and trace Elements since 2004. His primary research interest is in developing rapid analytical methods for small-molecule contaminants in foods using mass spectrometry. Prior to joining Symbiotic Research in 2016, Alex was Chief of the Bioanalytical Methods Branch in the Office of Regulatory Science at the US FDA’s Center for Food Safety and Applied Nutrition until his retirement in 2016. Prior to joining FDA in 2002, he worked for 12 years at EPA and 16 years for the U.S. Fish and Wildlife Service. In addition to his current work at Symbiotic Research, he also serves as a Science Adviser for the FDA’s Office of Research Coordination and Evaluation, in the Office of Regulatory Science, which is part of the Office of Regulatory Affairs. Altogether, he has 44 years of experience in his field.

Topic Background:

Liquid chromatography with tandem mass spectrometry (LC–MS/MS) is a powerful tool for the analysis of chemical residues in food. For example, given that the pesticides registered over the last decade are mostly polar compounds that are not always amenable to gas chromatographic techniques, LC–MS/MS is the methodology of choice to monitor these contaminants in foods for enforcement purposes. Likewise, LC–MS/MS is needed for the reliable determination of other polar food contaminants such as mycotoxins, veterinary drugs, and melamine and its analogs.

However, even though LC–MS/MS offers excellent sensitivity, selectivity, and overall speed of analysis, there are many important considerations which must be kept in mind when developing reliable methods for chemical residue analysis that rely on this technology. Some of these critical considerations include sample preparation; ways to compensate for matrix effects for accurate quantitation; mass spectrometry identification criteria (low-resolution versus high-resolution mass spectrometry); spiking of test portion versus incurred residue analysis; ruggedness; and the use of standard reference materials (if available) or proficiency test samples.

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