Food Testing & Environmental Analysis - Application Compendium

Importance of the topic

The analysis of trace contaminants and residues in food and environmental matrices is critical for public health, regulatory compliance, and quality control. Ultra‐trace detection of pesticides, sterilants, volatile phenols, and emerging contaminants such as 1,4‐dioxane requires highly sensitive, selective, and robust analytical platforms. Agilent Triple Quadrupole GC/MS systems, coupled with advanced sample preparation techniques, address these challenges by delivering low limits of quantitation, high throughput, and reliable routine performance.

Objectives and overview

This compendium presents a series of application studies that showcase the capabilities of Agilent Triple Quadrupole GC/MS systems (7000C, 7000D, 7010B) and GC instruments (8890, 7890B) for food and environmental testing. Key goals include:

• Quantitation of ethylene oxide and marker ethylene chlorohydrin in sesame seeds at 10 ppb.
• Low‐level multiresidue pesticide analysis in milk down to 1 ng/mL.
• Enhancement of SPME headspace extraction using salt addition for flavor and smoke impact compounds.
• Determination of free volatile phenols in smoke‐impacted wines by SPME‐GC/MS/MS.
• Trace analysis of 1,4‐dioxane in water via purge‐and‐trap GC/MS/MS to sub‐µg/L levels.
• Full‐scan quantitative screening of semivolatile organic compounds (SVOCs) with GC/TQ, demonstrating library matching and sensitivity comparable to single quadrupole GC/MS.

Methodology and instrumentation

Sample preparation approaches varied by application: liquid–liquid extraction and QuEChERS cleanup for sesame, milk multiclass extraction with EMR‐Lipid cartridges, salt‐spiking for SPME headspace, purge‐and‐trap for water, and full‐scan injection for SVOCs. Instrument platforms included:

• Agilent 8890 GC or 7890B GC with Multimode Inlet (MMI) or split/splitless (SSL) inlet.
• Agilent 7000C, 7000D, or 7010B Triple Quadrupole MS with high‐efficiency source (HES) or extractor EI source.
• SPME Arrow DVB/carbon WR/PDMS fibers for volatile phenols.
• Teledyne Tekmar Atomx XYZ purge-and-trap concentrator for water analysis.
• Agilent MassHunter software with spectral deconvolution, retention time locking, and automated MRM method generation.

Main results and discussion

The application studies achieved the following performance:

• Sesame seeds: LOQ of 10 ppb for ethylene chlorohydrin (marker of ethylene oxide) with S/N > 2.9, linearity R² > 0.998, and recovery 82–101%.
• Milk multiresidue pesticides: 8890/7010B achieved 1 ng/mL detection for ~60% of compounds, 7890B/7000C detected ~10% at 1 ng/mL, both systems linear to R² > 0.99.
• SPME headspace: addition of 4 g NaCl to 10 mL sample increased response for guaiacol and 4-methylguaiacol by 94–96%, improving sensitivity and repeatability (RSD < 11%).
• Smoke‐impacted wines: SPME‐GC/TQ quantified free volatile phenols (LOQ < 0.2 ppb), with calibration R² > 0.99 in Milli-Q water and wine matrices, and recovery within ±10%.
• 1,4-Dioxane in water: Purge-and-trap GC/TQ in dMRM delivered an MDL of 0.0198 µg/L, linear range 0.1–10 µg/L, accuracy 95–105%, with robust QC (CCV, LCS & LCSD meet EPA criteria).
• Full‐scan SVOCs: GC/TQ in full scan (35–500 m/z, 220 ms) produced average library match scores of 95 (NIST), LODs < 50 pg/µL for most targets, chromatographic resolution of benzo[b]/benzo[k]fluoranthene < 50%, and linear calibration (0.4–100 ppm) R² > 0.99.

Benefits and practical applications

These methods demonstrate several advantages:

• Enhanced sensitivity and selectivity using triple quadrupole MS/MS or optimized full-scan acquisition, enabling compliance with stringent regulatory limits.
• Reduced matrix interference through selective transitions (dMRM), retention time locking, and tailored sample cleanup.
• Increased throughput via automation (SPME autosamplers, purge-and-trap autosamplers) and reduced analysis time.
• Workflow flexibility to screen, confirm, and quantify a broad range of analytes in diverse food and environmental samples.

Future trends and possibilities

Emerging developments include:

• Integration of high-resolution accurate-mass GC/MS for non-target screening and metabolomics.
• Advanced software tools with AI-driven deconvolution and automated library matching for complex matrices.
• Miniaturized and field-deployable purge-and-trap and SPME systems for on-site monitoring.
• Expansion to novel contaminants, such as ultratrace PFAS, microplastics markers, and emerging disinfection byproducts.
• Continued improvement in source design and ion optics for even greater sensitivity and robustness.

Conclusion

The Agilent Triple Quadrupole GC/MS platforms, combined with tailored sample preparation techniques, deliver robust, sensitive, and selective solutions for food and environmental analysis. This compendium illustrates how optimized methods achieve low detection limits, high linearity, and reliable quantitation across diverse applications, supporting regulatory compliance and quality assurance.

Reference

1. Tateo F.; Benoni M. J. Food Compos. Anal. 2006, 19, 83–87.
2. Indian Oil Seeds and Produce Export Promotion Council, Procedure for Control of Contamination of Salmonella and Residues Including Ethylene Oxide in Sesame Seeds for Export to EU, 2020.
3. Yang X.; Zhang Y. Analysis of Multiclass Multiresidue Pesticides in Milk Using Agilent Captiva EMR—Lipid with LC/MS/MS and GC/MS/MS, Agilent Application Note 5994-2038EN, 2020.
4. Westland J.; Abercrombie V. Analysis of Free Volatile Phenols in Smoke-Impacted Wines by SPME, Agilent Application Note 5994-3161EN, 2021.
5. Westland J. Use of Salt to Increase Analyte Concentration in SPME Headspace Applications, Agilent Application Note 5994-3159EN, 2021.
6. U.S. EPA Method 8260D: Volatile Organic Compounds by GC/MS, Revision 3, 2006.
7. U.S. EPA Method 522: Determination of 1,4-Dioxane in Drinking Water by SPE and GC/MS with SIM.
8. U.S. EPA Method 8270E: Semivolatile Organic Compounds by GC/MS, Revision 6, 2018.
9. Churley M.; Quimby B.; Andrianova A. A Fast Method for EPA 8270 in MRM Mode Using the 7000 Series Triple Quadrupole GC/MS, Agilent Application Note 5994-0691EN, 2019.