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Screening for Pesticides in Food Using the Japanese Positive List Pesticide Method: Benefits of Using GC/MS with Deconvolution Reporting Software and a Retention Time Locked Mass Spectral Database

Applications | 2007 | Agilent TechnologiesInstrumentation
GC/MSD, GC/SQ
Industries
Food & Agriculture
Manufacturer
Agilent Technologies

Summary

Significance of the Topic


The Japanese Positive List system implemented in 2006 mandates strict maximum residue limits for pesticides in food, raising the need for fast and reliable analytical screening.
Comprehensive detection of over 430 GC-amenable pesticides is essential for regulatory compliance and consumer safety.

Objectives and Study Overview


The aim is to develop an automated, two minute per sample GC/MS screening method for 430 pesticides listed under the Japanese system.
The method integrates retention time locked mass spectral databases with deconvolution reporting software to identify trace residues in diverse food matrices.

Methodology and Instrumentation


Sample preparation uses QuEChERS extraction for fruit and vegetable matrices.
Analysis is performed on an Agilent 7890A GC coupled to a 5975C MSD operating in full scan mode (45–550 u) with a DB-5MS column under a retention time locked method calibrated to chlorpyrifos-methyl at 13.443 min.
Deconvolution Reporting Software (DRS) combines AMDIS spectral deconvolution and NIST05 library searching to extract clean spectra, match to a custom 430-compound pesticide library and the full NIST05 database for confirmation.

Main Results and Discussion


Screening of spiked strawberry and mixed fruit extracts demonstrated identification of seven of eight target pesticides at 500 ng/g levels within two minutes.
Deconvolution revealed low level pesticides such as azinphos-methyl coeluting with complex matrix peaks, which conventional library search missed.
Retention time locking ensured narrow time windows (±10 s) for high confidence identifications and minimal false positives.

Benefits and Practical Applications


The fully automated workflow reduces analyst dependency and processing time compared to manual SIM or multiple batch methods.
It provides rapid, comprehensive screening for regulatory compliance and import monitoring in food safety laboratories.
Average response factors enable approximate quantitation when full calibration is impractical.

Future Trends and Opportunities


Expansion to include LC-amenable pesticides will broaden coverage.
Integration with high resolution MS and advanced chemometric algorithms can improve sensitivity and reduce false negatives.
Global harmonization of retention time locking databases may facilitate interlaboratory method transfer.

Conclusion


The combination of retention time locked GC/MS and deconvolution reporting software delivers a rapid, robust, and comprehensive pesticide screening method suited to the Japanese Positive List requirements.
This approach enhances confidence in detections, minimizes manual review and supports high throughput food safety testing.

References


  • Department of Food Safety Ministry of Health Labour and Welfare Introduction of the Positive List System for Agricultural Chemical Residues in Foods 2006
  • Ministry of Health Labour and Welfare Positive List System for Agricultural Chemical Residues in Foods 2006
  • Japan Food Chemical Research Foundation Maximum Residue Limits List of Agricultural Chemicals in Foods
  • Ministry of Health Labour and Welfare Section A General Compositional Standards for Food Maximum Residue Limits of Substances Used as Ingredients of Agricultural Chemicals in Foods
  • Ministry of Health Labour and Welfare Section A General Compositional Standards for Food Provisional MRLs List
  • Department of Food Safety Ministry of Health Labour and Welfare Analytical Methods for Residual Compositional Substances of Agricultural Chemicals Feed Additives and Veterinary Drugs in Food
  • Lehotay SJ de Kok Hiemstra van Bodegraven QuEChERS Method J AOAC Int 88 595 614 2005
  • Anastassiades Lehotay Štajnbaher Schenck QuEChERS J AOAC Int 86 412 431 2003
  • Giarocco Quimby Klee Retention Time Locking Concepts and Applications Agilent Technologies 2007
  • Prest Wylie Weiner Agnew Efficient Screening for Pesticides and Endocrine Disrupters Using the 6890/5973 GC/MSD Agilent Technologies 2006
  • Wylie Screening for 926 Pesticides and Endocrine Disruptors by GC/MS with Deconvolution Reporting Software and a New Pesticide Library Agilent Technologies 2006
  • Quimby Screening for Hazardous Chemicals in Homeland Security and Environmental Samples Using a GC/MS/ECD/FPD with a 731 Compound DRS Database Agilent Technologies 2006
  • Szelewski Quimby New Tools for Rapid Pesticide Analysis in High Matrix Samples Agilent Technologies 2005
  • Sandy A Blind Study of Pesticide Residues in Spiked and Unspiked Fruit Extracts Using Deconvolution Reporting Software Agilent Technologies 2005
  • Wylie Szelewski Meng Sandy Comprehensive Pesticide Screening by GC/MSD Using Deconvolution Reporting Software Agilent Technologies 2005
  • Ping Meng Szelewski Building Agilent GC/MSD Deconvolution Reporting Libraries for Any Application Agilent Technologies 2006
  • Lesueur Gartner Routine Identification and Quantification of Pesticide Multiresidues in Fruit and Vegetable Samples with Full Scan SIM and Deconvolution Reporting Software Ernährung Nutrition 29 466 471 2005
  • Hirahara et al Validation of Multiresidue Screening Methods for the Determination of 186 Pesticides in 11 Agricultural Products Using Gas Chromatography J Health Science 51 617 627 2005
  • Ministry of Health Labour and Welfare Imported Foods Monitoring Plan for 2006 Notices Nos 0331006 and 0525001 2006

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