Best practices for food safety laboratories: highlights from inaugural Agilent—AOAC workshop
Thierry Faye Agilent Global Market Development Manager
Chandrasekar Kandaswamy Agilent GC/MS Senior Market Development Scientist
Anand Sheshadri Agilent LC/MS Senior Market Development Scientist
Ankur Srivastava Agilent Market Program Manager
Food safety is a topic of concern to all of us, and Agilent collaborates with leading scientists from governmental and industrial organizations around the world to improve the safety and quality of food. Agilent and the India section of AOAC International (Association of Analytical Communities) organized a two-day training workshop in India for food scientists on best practices from European Union (EU) guidelines (SANTE 11945/2015).
Thank you Agilent for organizing such a professional and information-rich exchange program. Having access to EU experts on food regulations as well as your most recent products and workflows is key to the success of our food safety mission.
Dr. Kaushik Banerjee, President of the India section of AOAC International
Figure 1. Dr. Carmen Amate presented helpful information about EU guidelines for pesticide method validation.
The workshop agenda included a balance of lectures, hands-on training, and discussions. The practical laboratory sessions provided the opportunity to demonstrate sample preparation (in particular our successful QuEChERS solutions). They also included method optimization and troubleshooting on Agilent triple quadrupole 7010B GC/MS and 6945 LC/MS, as well as on the 7800 ICP-MS.
Fulfill European Union guidelines
Dr. Carmen Ferrer Amate from the EURL (European Reference Laboratory) for pesticides in fruits and vegetables (Almeria, Spain) shared her expertise with the workshop attendees on the most relevant method validation parameters to meet European Union guidelines (Figure 1). She discussed matrix effects for various foodstuffs relative to LC/MS/MS and GC/MS/MS quantification and explained how to overcome enhancement or suppression of signal by using dilution techniques or cleanup procedures like Agilent QuEChERS Enhanced Matrix Removal—Lipid for fatty matrices.
“We always enjoy working with Agilent instruments, columns, and sample preparation material, as they simply deliver excellent results over the long run,” said Dr. Carmen Ferrer Amate. She concluded with a presentation on the EURL network activities and proficiency tests (EUPTs).
Optimize sample preparation to get best chromatographic results
Ram Prasad Ganni, Agilent Product Specialist, explained the importance of sample preparation in food contaminant testing and the challenges in various food matrices. He explained the merits of various sample preparation techniques for analysis of food contaminants. For solid phase extraction (SPE) and QuEChERS techniques, he described the importance of each sample processing step and its influence on chromatography and recoveries. A hands-on extraction and dispersive cleanup of chili demonstrated how to improve chromatographic results and decrease instrument downtime with optimized sample preparation.
Figure 2. Overlaid chromatograms show very good consistency for the 50 ng/mL GC/MS pesticide analysis calibration check (blue) after 60 honey extract injections (red), and after liner and Agilent Intuvo Guard Chip replacement (green).
Quickly build acquisition methods that reduce matrix interferences
Agilent GC/MS Scientist Chandrasekar Kandaswamy emphasized the importance of lab-to-lab result reproducibility and impact of the selection of MRM transitions in multi-residue quantification. Sample preparation was optimized with a modified QuEchERS technique to minimize co-extractives and to achieve recoveries in the 70 to 120 percent range (Figure 2). Use of Retention Time Locking and the Agilent MassHunter Pesticide and Pollutant MRM Database saved time when setting up GC/MS/MS instrumental parameters. With the availability of an average of five MRM transitions for 1100 pesticides—polychlorinated biphenyls (PCBs), and polycyclic aromatic hydrocarbons (PAHs)—it was possible to choose matrix-free MRM transitions for targeted compounds and achieve superior selectivity for routine analysis.
Quantify trace metals and other elements in food
Dr. Vinay Jain, Agilent ICP-MS Application Chemist, discussed the Solution-Ready Agilent 7800 ICP-MS, which combines proven, robust hardware, auto-optimization tools, and preset methods to simplify routine analysis, making your laboratory more productive and your results more reliable. Even more important, with high matrix tolerance, wide dynamic range, and effective control of polyatomic interferences, the Agilent 7800 ICP-MS takes the uncertainty out of analysis of complex or variable sample matrices. The 7800 ICP-MS is extraordinarily easy to set up and use, so you can quickly produce reliable results in the widest range of sample matrices, such as food and farm products. As proof, Dr. Jain demonstrated trace metal analysis and quantification in milk powder.
Figure 3. The workshop provided opportunities for fruitful discussions. Dr. Thierry Faye, Agilent (left), and Dr. K. K. Sharma, Network Coordinator of All India Network Project on Pesticide Residues, Indian Agricultural Research Institute (right), share their collective experiences.
Save time with a single LC/MS/MS method for 275 analytes
Anand Sheshadri, Agilent LC/MS Scientist, described development of a single LC/MS method for screening and quantification of trace levels of pesticides, mycotoxins, dyes, and pyrrolizidine alkaloids (PAs) in spice samples. A simple Enhanced Matrix Removal-QuEChERS sample cleanup technique was effectively used for chili and turmeric samples prior or LC/MS analysis. About 245 pesticides, 20 PAs, 6 dyes, and 4 aflatoxins were analyzed with a single LC/MS/MS method. Quantitation of analytes was performed with matrix-matched calibration standards. The analysis took advantage of the Agilent 1290 Infinity II LC System as a front end to an Agilent 6495 Triple Quadrupole LC/MS. More than 75 percent of the analytes showed good recoveries in the 70 to 130 percent range.
Ensure safer food
The food and agriculture industry faces ever-increasing demands for highly sensitive and productive analytical solutions. Ongoing collaborative workshops provide the tools and techniques to tackle these challenges (Figure 3).
Dr. Carmen Amate presented helpful information about EU guidelines for pesticide method validation.
Overlaid chromatograms show very good consistency for the 50 ng/mL GC/MS pesticide analysis calibration check (blue) after 60 honey extract injections (red), and after liner and Agilent Intuvo Guard Chip replacement (green).
The workshop provided opportunities for fruitful discussions. Dr. Thierry Faye, Agilent (left), and Dr. K. K. Sharma, Network Coordinator of All India Network Project on Pesticide Residues, Indian Agricultural Research Institute (right), share their collective experiences.