Shimadzu Food Safety Management Data Book

Importance of Topic

Pesticide residues in foods and agricultural products pose critical safety and regulatory challenges worldwide. Reliable methods capable of detecting trace levels of dozens to hundreds of compounds are essential for consumer protection, trade compliance, and environmental monitoring. Recent advances in instrumentation and sample-prep automation have greatly expanded the scope, speed, and sensitivity of multi-residue analysis.

Objectives and Overview

The document C219-E007A provides a comprehensive compendium of validated analytical methods for residual pesticides and related contaminants. It covers:

• Multi-residue screening of 124 pesticides by capillary GC with flame photometric and electron-capture detection.
• Simultaneous analysis of organophosphorus, organochlorine, and pyrethroid pesticides by GC/MS (EI and NCI modes).
• Analysis of polar and thermally labile pesticides using LC, LC/MS (ESI and APCI), and post-column derivatization.
• Sample pretreatment strategies including liquid–liquid extraction, solid-phase extraction, gel permeation chromatography (GPC), and fully automated GPC–GC/MS (Prep-Q).
• Methods for veterinary drugs, food additives, mycotoxins, inorganic contaminants, and reference materials.

Methodology and Instrumentation

The key techniques and instruments include:

• Capillary GC-FTD/ECD: Four stationary phases (DB-1, DB-5, DB-1301, DB-17) with tailored temperature programs for 124 pesticides; high-pressure splitless injection; relative retention indices for rapid screening.
• GC/MS (EI and NCI): SIM and scan modes for simultaneous detection of 80+ pesticides at sub-µg/kg levels; NCI enhances selectivity for chlorinated analytes.
• GC/MS On-line GPC (Prep-Q): Automated coupling of GPC clean-up with GC/MS; half the analysis time and solvent consumption of conventional rapid methods.
• HPLC and LC/MS: High-resolution FC-ODS and VP-ODS columns; UV, fluorescence, and photodiode-array detection; ESI- and APCI-MS for polar, thermally labile, and metabolite profiling.
• Post-column derivatization: Fluorescent tagging with OPA for carbamate analysis; enzymatic and chemical hydrolysis for total residue determination.

Main Results and Discussion

• GC-FTD/ECD methods achieved baseline separation for 124 pesticides across multiple capillary phases; retention time libraries enable fast screening.
• GC/MS methods demonstrated linear response (R2>0.999) and repeatability (CV<5%) for dozens of compounds, with detection limits down to low ppb.
• NCI provided 5–10× sensitivity improvements over EI for chlorinated pesticides and enabled trace quantification in complex matrices.
• On-line GPC–GC/MS (Prep-Q) automated the entire clean-up and analysis workflow, reducing per-sample time from 170 min to 80 min and solvent usage by >90%.
• LC/MS workflows delivered multi-residue screening of veterinary drugs and phenoxy-acid herbicides with positive/negative ion switching and sub-ng injection sensitivity.

Benefits and Practical Applications

• Standardized multi-residue methods streamline laboratory operations for routine QA/QC in food safety, environmental, and regulatory labs.
• Automation via on-line GPC and multi-sequence LC/MS reduces hands-on time, improves throughput, and minimizes human error.
• NCI and LC/MS expand the analytical window to ultra-trace levels and thermally labile or highly polar compounds.
• Comprehensive method coverage (pesticides, veterinary drugs, additives, mycotoxins, metals) supports integrated safety assessment.

Future Trends and Opportunities

• Further integration of sample-prep automation (online SPE-LC/MS, robotic GPC) to achieve true walk-away workflows.
• High-resolution accurate mass spectrometry for non-targeted screening and retrospective data mining of emerging contaminants.
• Miniaturized and portable GC/MS and LC/MS instruments for field and point-of-use testing.
• Advanced data analytics, machine learning, and spectral libraries for rapid peak identification and false-positive reduction.
• Expansion of multi-residue panels to new pesticide chemistries, degradation products, and novel agrochemicals.

Conclusion

C219-E007A represents a state-of-the-art reference for multi-residue analysis of pesticides and related contaminants in foods and agricultural products. By combining selective detection, robust separation, and automated clean-up, these methods meet stringent regulatory requirements while maximizing laboratory efficiency. Ongoing innovation in instrumentation and data processing will further enhance our ability to safeguard food safety and environmental health.

References

• Ministry of Health, Labour and Welfare (Japan), Notification No. 370: Rapid Analysis Method for Residual Pesticides (1997).
• Environmental Health Bureau, Food Chemistry Division (Japan), Notices 43, 44, 45: Pesticide-Residue Rapid Analysis Method (1997).
• Shimadzu Application Notes and C219-E007A Technical Manual.