Mass Spectrometry Applications for Food Safety Analysis

Importance of Topic

The routine surveillance of pesticide residues in food and beverages is essential for consumer safety and regulatory compliance. As agricultural practices intensify and global trade expands, a diverse range of matrices—fruit preserves, produce, processed juices and complex beverages—require rapid, sensitive and reliable analytical solutions to detect contaminants at or below statutory limits.

Objectives and Overview of Study / Article

This collection of application studies demonstrates the development and validation of multi-residue pesticide methods in various food matrices:

• Rapid multi-residue analysis of 96 priority pesticides in fruit jam using a QuEChERS extraction and GC-MS/MS (Thermo Scientific TSQ Quantum XLS).
• High-throughput screening of 250 pesticides in onion matrix by rapid-scan LC-MS/MS (Thermo Scientific TSQ Quantiva) employing a Q2 drag field for 500 SRMs/sec acquisition.
• Determination of 24 fungicide residues in red wine via QuEChERS sample prep, dispersive SPE cleanup and LC-MS/MS on Accucore aQ columns with a TSQ Vantage.
• Automated online cleanup of carbendazim and benomyl in oranges and orange juice using Transcend TLX turbulent flow extraction coupled to LC-MS/MS (TSQ Quantum Access MAX).

Methodology and Instrumentation

All methods leverage tandem quadrupole mass spectrometry, combining selective reaction monitoring with tailored sample preparation:

• QuEChERS protocols with citrate or acetate buffers, acetonitrile extraction and PSA/MgSO4 dSPE for jam and red wine matrices.
• Splitless or large-volume GC-MS/MS with TR-Pesticide capillary column for semi-volatile residues in polar acetonitrile extracts.
• Fast LC gradients on Core Enhanced Technology™ columns (Accucore aQ and Hypersil GOLD) for polar and non-polar analytes in aqueous matrices.
• TurboFlow™ (Transcend TLX) online cleanup to exclude macromolecules, followed by direct transfer to analytical column for automated orange juice analysis.
• High-rate SRM acquisition using a Q2 drag field in TSQ Quantiva enabling 500 SRMs/sec at 1 ms dwell time for onion screening.

Key Results and Discussion

Across matrices, validated methods met or exceeded performance criteria:

• Limits of quantitation typically ≤ 0.005–0.01 mg/kg, well below EU default MRLs (0.01 mg/kg) and US action limits.
• Linearity coefficients (r2) > 0.98–0.999 across multi-point matrix-matched curves.
• Recovery rates of 70–120% with relative standard deviations < 15% for ≥ 90% of analytes in jam, wine and oranges.
• High selectivity demonstrated by clear SRM traces and consistent ion ratios in complex backgrounds.
• Fast total run times: 57 min GA-MS/MS for 96 pesticides in jam, 13 min TLX-LC-MS/MS in oranges, 20 min LC-MS/MS in wine, and 45 min LC–MS/MS screening of 250 pesticides in onion.
• Enhanced throughput: > 100 samples/day for TLX workflow, and simultaneous monitoring of hundreds of SRMs in onion screening.

Benefits and Practical Applications of the Methods

These tailored approaches improve routine testing capabilities:

• Reduced sample handling and solvent use via online cleanup and QuEChERS, lowering costs and environmental impact.
• Automated workflows (TLX coupling) minimize manual errors and increase laboratory efficiency.
• High-speed SRM acquisition expands the number of monitored pesticides without compromising sensitivity.
• Compatibility with regulatory guidelines (EU DG SANCO, US FDA) ensures reliable MRL compliance checks.
• Flexibility to adapt to diverse matrices—from sticky fruit preserves to high-pigment wines and acidic juices.

Future Trends and Opportunities

Advances in food safety analysis will focus on:

• Integration of ultra-high-throughput instrumentation (faster quadrupoles, ion mobility, high-resolution MS) for comprehensive screening of thousands of compounds.
• Further automation in sample preparation, including robotics and online solid-phase microextraction for complex and solid samples.
• Green analytical chemistry: miniaturized extraction methods, reduced solvent volumes and re-usable sorbents.
• Data-driven quality control with real-time analytics and cloud-based reporting to enhance traceability in global supply chains.

Conclusion

The combination of targeted sample preparation strategies (QuEChERS, TurboFlow TLX) with robust GC-MS/MS and LC-MS/MS platforms provides rapid, sensitive and reproducible pesticide residue analysis in challenging food matrices. These validated workflows meet stringent regulatory requirements, support high-throughput monitoring and offer a strong foundation for next-generation food safety testing.

References

1 Regulation (EC) No 396/2005 on MRLs of pesticides in food.
2 US FDA action limit guidance for carbendazim in orange juice.
3 Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ. AOAC Int. 2003, 86(2):412–431.
4 European Commission DG SANCO document SANCO/10684/2009.
5 Hajšlová J, et al. J. Chromatogr. A. 1998, 800:283–295.
6 Godula M, et al. J. High Resol. Chromatogr. 1999, 22(7):395–402.
7 Thermo Fisher Scientific application notes: AN51880, AN20830, ASMS13_T602.
8 AOAC and IUPAC single-laboratory validation guidelines.