Advances in Food Testing & Environmental Analysis - Application Compendium

Importance of Microanalysis in Food and Environmental Testing

Modern analytical challenges in food safety and environmental monitoring demand highly sensitive, selective, and robust methods for trace contaminants. Compounds such as monochloropropanediol esters, 1,4-dioxane, smoke-taint phenols, volatile organic compounds in soils, dioxins/furans, and microplastics require tailored sample preparation and instrumentation. Accurate quantitation of these analytes protects public health, supports regulatory compliance, and guides remediation strategies.

Objectives and Overview of Studies

Seven application studies examined analytical workflows using advanced gas chromatography–mass spectrometry (GC-MS) platforms. Key goals included:

• Determining MCPD esters in infant formula via indirect cleavage and derivatization (HFBI or PBA) with GC/MSD.
• Quantifying 1,4-dioxane in cosmetics and household products by headspace GC/MS.
• Measuring smoke-impact volatile phenols in wines using SPME-GC/MS/MS.
• Enhancing SPME extraction by salt addition for improved headspace yields.
• Comparing SPME Arrows and fibers for volatile phenol analysis.
• Analyzing soil and sediment VOCs via headspace GC/MS using the Agilent 8697 sampler.
• Developing an Agilent 7010B Triple Quadrupole GC/MS alternate method for EPA 1613B dioxins/furans analysis.
• Implementing automated TED-GC/MS for microplastic polymer identification and quantitation.

Methodology and Instrumentation

All studies leveraged Agilent GC platforms and MS detectors: 5977B GC/MSD, 7000D/7010B Triple Quadrupole, and high-throughput headspace (7694E/7697A). Sample preparation techniques included QuEChERS extraction and SPE cleanup for food matrices, SPME fibers and Arrows for volatile phenols, saturated NaCl addition for enhanced headspace extraction, and thermal extraction/desorption coupled to TGA for microplastics. Derivatization reagents (HFBI, PBA) and isotope dilution internal standards ensured selectivity and quantitation accuracy.

Main Results and Discussion

• MCPD esters: Excellent linearity (R2>0.997), recoveries 87–107%, MDL ~1.3 μg/kg.
• 1,4-Dioxane: Headspace GC/MS yielded LODs of 2.3–7.1 ppb; seven-point calibration 6.5 ppb–20 ppm.
• Volatile phenols: SPME/GC/MS/MS in wines delivered LOQs <0.1 ppb and recoveries 80–120%.
• Salt addition in headspace-SPME doubled analyte signals for smoke phenols.
• SPME Arrows boosted extraction efficiency by 4–7× over fibers for phenol compounds.
• Soil VOCs: Agilent 8697 headspace sampler achieved area precision 1–4.3%, LODs 0.51–1.21 µg/kg, recoveries 72–126%, R2≥0.996.
• Dioxins/furans: Agilent 7010B TQ GC/MS matched EPA 1613B performance in sensitivity, linearity, MDLs, and reference material accuracy.
• Microplastics: Automated TED-GC/MS detected polymers at 0.06–2.2 µg sample mass, repeatability RSD 6–12%, analyzing up to 1 g in under 2.5 hours.

Benefits and Practical Applications

These workflows enable laboratories to:

• Meet regulatory limits for contaminants in food, cosmetics, and environmental samples.
• Improve throughput through automation (headspace, SPME, TED-GC/MS) and reduce solvent usage.
• Quantify all relevant size fractions, from ppb to ppm levels.
• Switch from high-cost HRMS to GC/MS/MS platforms while maintaining data quality.

Future Trends and Opportunities

Ongoing developments include coupling GC/MS with machine-learning data analysis, expanding microplastic polymer libraries, and integrating multi-dimensional GC for complex matrices. Miniaturized and portable GC/MS systems promise on-site screening capabilities. Further method harmonization will facilitate broader environmental monitoring networks.

Conclusion

Advanced GC/MS techniques, including SPME, headspace sampling, GC/TQ, and TED-GC/MS, offer reliable, high-throughput, and cost-effective solutions for trace analysis of complex food and environmental contaminants. These methods support regulatory compliance, environmental protection, and food safety initiatives by providing accurate, reproducible data across diverse matrices.

References

• Ahn, T.; et al. MCPD Esters in Infant Formula by GC/MSD. Application Note. 2021.
• Fernando, S.; Haddad-Carroll, A. 1,4-Dioxane by Headspace GC/MS. Application Note. 2021.
• Westland, J.; Abercrombie, V. Smoke-Impact Phenols by SPME-GC/MS/MS. Application Note. 2021.
• Westland, J. Salt Enhancement in SPME Headspace. Application Note. 2021.
• Westland, J. SPME Arrows vs. Fibers for Phenols. Application Note. 2021.
• Zhang, J.; et al. Soil VOCs Using Agilent 8697 Headspace. Application Note. 2021.
• Hamilton, C.; et al. Alternate EPA 1613B with Agilent GC/TQ. Application Note. 2021.
• Braun, U.; et al. Automated TED-GC/MS for Microplastics. Application Note. 2020.