An integrated GC-MS/MS and LC-MS/MS workflow for quantitative analysis of pesticides with cross- confirmation using a single chromatography data system software

Importance of the topic

Modern agriculture relies on hundreds of pesticides to protect crops and secure food supply. Monitoring trace levels of these compounds in food matrices is essential to meet regulatory limits, safeguard consumer health, and support trade. An integrated workflow combining gas chromatography tandem mass spectrometry and liquid chromatography tandem mass spectrometry enhances detection scope, accuracy, and laboratory efficiency in multi residue pesticide analysis.

Objectives and study overview

This study evaluated the performance of an out of the box pesticide analysis solution using a single chromatography data system for cross confirmation. Proficiency test samples of wheat and green beans containing a mixture of up to 25 unknown pesticides were analyzed. The goals were to demonstrate accurate quantitation, rapid identification confirmation, and streamlined data review using an integrated software interface.

Methodology and instrumentation

Sample Preparation

• Green beans and wheat samples spiked with 10 to 25 pesticides at 0.02 to 0.2 mg/kg were extracted by QuEChERS AOAC 2007.01.
• Extracts for LC MS MS were directly injected; GC MS MS extracts underwent cleanup and solvent exchange to heptane.

Instrumentation

• Liquid chromatography: Vanquish Flex UHPLC with Hypersil GOLD C18 column coupled to Altis Plus triple quadrupole.
• Gas chromatography: TRACE 1610 GC with TriPlus SMART autosampler, iConnect Thermospray injector, AEI source, and TSQ 9610 triple quadrupole, using TraceGOLD TG SQC column.
• Data system: Chromeleon CDS version 7.3.2 with cross confirmatory user interface and preconfigured pesticide workflows.

Main results and discussion

All detected pesticides in wheat and green bean proficiency tests fell within regulatory limits, with Z scores predominantly below one and satisfactory classification. Cross confirmation between GC MS MS and LC MS MS reduced false positives and false negatives and eliminated the need for re analysis. Customized view settings guided analysts through retention time, calibration, QC, internal standard, and ion ratio checks, improving review consistency and reducing training time.

Benefits and practical applications

The integrated workflow delivers:

• Comprehensive multi residue capability for up to 700 pesticides.
• Increased confidence in results through automated cross confirmation.
• Reduced method development and training overhead via pre configured acquisition and processing templates.
• Efficient data management on a single workstation or enterprise network.

Future trends and opportunities

Emerging developments may include expanded analyte libraries, AI driven data review, cloud based chromatography data systems for global collaboration, and further instrument automation. Integration of high resolution mass spectrometry and machine learning algorithms could enhance identification of novel pesticide metabolites and contaminants.

Conclusion

The unified GC MS MS and LC MS MS solution with cross confirmatory software provides accurate, precise, and reliable multi residue pesticide analysis. Its out of the box configuration streamlines laboratory workflows, supports regulatory compliance, and reduces operational burden while maintaining high data quality.

References

1. World Health Organization Pesticide residues in food Fact Sheet September 15 2022
2. European Commission Directorate General for Health and Safety Guidance on analytical quality control and method validation SANTE 11312 2021
3. Chromeleon CDS Pesticides Solution accessed January 11 2024
4. BIPEA Proficiency testing programs accessed January 11 2024
5. BIPEA Multi residue screening of pesticides Cereals and Vegetables