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Simultaneous Analysis of Pesticides in Food With GC-MS/MS Using Hydrogen Carrier Gas

Posters | 2024 | Shimadzu | AOACInstrumentation
GC/MSD, GC/MS/MS, GC/QQQ
Industries
Food & Agriculture
Manufacturer
Shimadzu

Summary

Significance of the topic


Multi-residue analysis of pesticides in food is essential for consumer safety and regulatory compliance. Helium is the traditional carrier gas for GC-MS/MS but recent supply shortages and price increases drive the search for alternatives. Hydrogen is a viable substitute offering cost savings and compatible performance for high throughput analysis.

Objectives and overview of the study


This study aims to develop and validate a quantitative GC-MS/MS method using hydrogen as carrier gas for simultaneous analysis of 216 pesticide residues in food matrices such as orange and spinach. Validation included recovery, repeatability and calibration performance.

Methodology


  • Samples of whole orange and spinach were freeze ground and extracted using QuEChERS AOAC 2007.01 protocol
  • Cleanup was performed with dispersive SPE dSEP tubes
  • Samples were spiked at 10 ng per mL to assess recovery and repeatability
  • Calibration standards ranged from 1 to 100 ng per mL for most compounds and up to 100 ng per mL for lower responding analytes

Instrumentation


  • GC-MS/MS system Shimadzu GCMS TQ8050 NX equipped with AOC 30i and AOC 20s U auto injectors
  • Column SH I 5Sil MS 30 m x 0.25 mm ID 0.25 microm stationary phase with Rxi guard column
  • Carrier gas hydrogen generated by Peak Scientific hydrogen generator at 60.5 cm per sec linear velocity
  • Temperature program initial 70C hold 1 min then 40C per min to 125C ramp 10C per min to 300C hold 20 min
  • Injection spitless 1 micro liter injector temperature 250C
  • MS detection electron ionization at EI 230C interface MRM data acquisition with 150 micro amp emission current

Main results and discussion


The method provided recovery rates within 70 to 120 percent for approximately 70 to 74 percent of the 216 target pesticides in orange and spinach. Repeatability expressed as relative standard deviation was below 10 percent for the majority of compounds. Calibration curves demonstrated linear response over the tested concentration ranges. Representative chromatograms confirmed clear separation and sensitivity.

Benefits and practical applications


  • Use of hydrogen reduces operational cost and dependence on helium supply
  • High sensitivity and rapid analysis support routine monitoring in food safety laboratories
  • Method covers a broad range of pesticide chemistries in a single run

Future trends and opportunities


Further extensions of this approach may include additional food matrices and environmental samples. Automation of sample preparation and adoption of advanced data processing tools such as artificial intelligence can enhance throughput. Emphasis on green chemistry may drive wider adoption of hydrogen and other sustainable carrier gases.

Conclusion


This work demonstrates that hydrogen can effectively replace helium in GC MS MS for multi residue pesticide analysis without compromising performance. The validated method delivers reliable recovery repeatability and sensitivity for over 200 pesticides and offers a viable solution to helium shortages.

References


No references were provided.

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