Fast, practical, and effective approach for the analysis of hazardous chemicals in the food supply
Authors: Lehotay Steven J. , Amirav Aviv 
Published: March 2022

Background to the topic: For food safety and security reasons, hundreds of pesticides, veterinary drugs, and environmental pollutants should be monitored in the food supply, but current methods are too time-consuming, laborious, and expensive. As a result, only a tiny fraction of the food is tested for a limited number of contaminants. Original proposal objectives: Our main original goal was to develop fast, practical, and effective new approaches for the analysis of hazardous chemicals in the food supply. We proposed to extend the QuEChERS approach to more pesticides, veterinary drugs and pollutants, further develop GC-MS and LC-MS with SMB and combine QuEChERS with GC-SMB-MS and LC-SMB-EI-MS to provide the “ultimate” approach for the analysis of hazardous chemicals in food. Major conclusions, solutions and achievements: The original QuEChERS method was validated for more than 200 pesticide residues in a variety of food crops. For the few basic pesticides for which the method gave lower recoveries, an extensive solvent suitability study was conducted, and a buffering modification was made to improve results for difficult analytes. Furthermore, evaluation of the QuEChERS approach for fatty matrices, including olives and its oil, was performed. The QuEChERS concept was also extended to acrylamide analysis in foods. Other advanced techniques to improve speed, ease, and effectiveness of chemical residue analysis were also successfully developed and/or evaluated, which include: a simple and inexpensive solvent-in-silicone-tube extraction approach for highly sensitive detection of nonpolar pesticides in GC; ruggedness testing of low-pressure GC-MS for 3-fold faster separations; optimization and extensive evaluation of analyte protectants in GC-MS; and use of prototypical commercial automated direct sample introduction devices for GC-MS. GC-MS with SMB was further developed and combined with the Varian 1200 GCMS/ MS system, resulting in a new type of GC-MS with advanced capabilities. Careful attention was given to the subject of GC-MS sensitivity and its LOD for difficult to analyze samples such as thermally labile pesticides or those with weak or no molecular ions, and record low LOD were demonstrated and discussed. The new approach of electron ionization LC-MS with SMB was developed, its key components of sample vaporization nozzle and flythrough ion source were improved and was evaluated with a range of samples, including carbamate pesticides. A new method and software based on IAA were developed and tested on a range of pesticides in agricultural matrices. This IAA method and software in combination with GC-MS and SMB provide extremely high confidence in sample identification. A new type of comprehensive GCxGC (based on flow modulation) was uniquely combined with GC-MS with SMB, and we demonstrated improved pesticide separation and identification in complex agricultural matrices using this novel approach. An improved device for aroma sample collection and introduction (SnifProbe) was further developed and favorably compared with SPME for coffee aroma sampling. Implications, both scientific and agricultural: We succeeded in achieving significant improvements in the analysis of hazardous chemicals in the food supply, from easy sample preparation approaches, through sample analysis by advanced new types of GC-MS and LCMS techniques, all the way to improved data analysis by lowering LOD and providing greater confidence in chemical identification. As a result, the combination of the QuEChERS approach, new and superior instrumentation, and the novel monitoring methods that were developed will enable vastly reduced time and cost of analysis, increased analytical scope, and a higher monitoring rate. This provides better enforcement, an added impetus for farmers to use good agricultural practices, improved food safety and security, increased trade, and greater consumer confidence in the food supply.