Application Handbook Food, Beverages, Agriculture - Release 2

Significance of Topic

Ensuring the safety and quality of food, beverages and agricultural products is critical to public health and industry compliance around the world. Analytical methods capable of detecting pesticide residues, veterinary drugs, mycotoxins, industrial contaminants and mineral oil hydrocarbons at trace levels are in growing demand as regulations tighten and consumer awareness rises. High-throughput, high-sensitivity instrumentation is needed to cover the diverse range of analytes encountered in complex matrices from cereals and baby food to beverages, oils and environmental samples.

Objectives and Study Overview

This Application Handbook compiles state-of-the-art approaches for the rapid, reliable and fully automated analysis of key contaminants in food, beverages and agricultural samples. It surveys chromatographic and mass spectrometric techniques including gas chromatography (GC), comprehensive two-dimensional GC (GC×GC), liquid chromatography (LC), supercritical fluid extraction (SFE) coupled to supercritical fluid chromatography (SFC) and tandem MS, as well as post-column reaction strategies. The handbook aims to demonstrate methods for multi-class, multi-residue screening and targeted quantification, highlighting enhanced sample preparation, improved separation, high-speed detection and regulatory compliance.

Methodologies and Instrumentation

• GC and GC×GC: Standard and silver-ion SPE cleanup precede GC-FID or GC-MS/MS/MS screening of pesticides, mineral oil saturated and aromatic hydrocarbons (MOSH/MOAH), polycyclic aromatic hydrocarbons and residual solvents. Comprehensive GC×GC with photodiode array or MS detection aids in profiling isomers and complex mixtures. Auto-adjustment of retention times and multi-column switching ensure robustness.
• LC-MS/MS: QuEChERS acetonitrile extraction and ligand-exchange or mixed-mode columns enable direct analysis of amino acids, sugars and veterinary drugs without derivatization. Ultra-high-performance LC coupled to triple-quadrupole MS (LCMS-8030, ‑8050) provides sub-ppb detection of mycotoxins, antibiotics and feed additives in dairy, meat and beverage matrices using fast polarity switching and matrix-matched calibration.
• LCMS-IT-TOF: High-resolution accurate-mass detection of industrial dyes, food colorants and complex lipid contaminants is achieved by reversed-phase and mixed-mode chromatography on APCI or ESI interfaces, enabling non-targeted screening with elemental composition data.
• SFE-SFC-MS: Supercritical CO₂ extraction with online trapping and gradient-modulated SFC delivers automated, solvent-reduced analysis of pesticide residues in agricultural products (FIFRA, MRL screening) with continuous sample handling and minimal carryover.
• Off-line SFE-GC/MS: Rapid, solvent-efficient extraction of pesticides and lipophilic contaminants from dry matrices followed by GC-MS/MS ensures robust quantification across broad analyte classes.

Main Results and Discussion

– GC-MS/MS methods achieved simultaneous quantification of over 300 pesticides at low ng/g in food matrices with high linearity (R²>0.99), matrix-matched calibration and minimal cleanup.
– GC×GC-MS profiling of MOSH/MOAH contaminants in produce and packaging materials allowed class-based separation, identification of fatty acid esters and quantification of migration levels against regulatory limits.
– LCMS methods quantified 45 mycotoxins in baby food at sub-ppb levels with fast gradient runs (<11 min) using positive/negative polarity switching and triple-quadrupole tandem MS.
– QuEChERS-based LC-MS/MS analysis of amino acids and sugars in beverages, dairy and spirits was performed without derivatization, with detection limits of 0.05–1 mg/L and excellent repeatability (<6% RSD).
– SFE-SFC-MS and off-line SFE-GC/MS systems demonstrated automated, high-throughput extraction and analysis of pesticide residues spanning polar and non-polar classes, achieving 70–120% recoveries with minimal sample handling.

Benefits and Practical Applications

– High-throughput, multi-residue methods reduce labor, solvent use and instrument runtime while meeting regulatory standards (EU MRLs, JECFA, FDA, Codex).
– Automated retention time adjustment and polarity switching streamline method setup and maintenance.
– Comprehensive 2D-GC and high-resolution TOF-MS enable non-targeted screening for emerging contaminants and food fraud.
– QuEChERS workflows coupled to LC-MS/MS expand analyte coverage with minimal cleanup.

Future Trends and Potential Applications

– Integration of online sample preparation (SFE, QuEChERS robots) with two-dimensional UHPLC and fast-scanning MS/MS for real-time monitoring and process control.
– Machine-learning enhanced chromatogram deconvolution for non-targeted contaminant surveillance.
– Eco-friendly, solvent-minimized SFC and universal detectors for lipidome and flavorome profiling.
– Standardization of high-resolution, high-speed LC-MS/MS protocols for emerging food contaminants, allergens and nutritional markers.

Conclusion

Advances in chromatography and mass spectrometry, together with streamlined sample preparation, now enable unprecedented throughput, sensitivity and selectivity for food and agricultural analysis. The methods presented facilitate comprehensive screening, targeted quantitation and non-targeted discovery of a wide range of contaminants in complex matrices, supporting compliance, risk assessment and quality control in global food supply chains.

Used Instrumentation

• Shimadzu GC-2010/GCMS-2020/GCMS-TQ8030 Triple-quadrupole GC/MS
• Shimadzu Nexera/Iq/UFLC LC-20AD/1200/LCMS-8050/LCMS-8030/LCMS-IT-TOF LC-MS/MS systems
• Shimadzu SFE-UC SFE-SFC-MS online and off-line extraction systems
• Shim-pack, Supelco, Restek, Rxi, InertCap, Ag-SPE, Myco-SPE, Silica SPE columns
• IT-TOF Software, ChromSquare, SmartMRM, AART, GCMSolution, LabSolutions Insight, LEChem

References

[1] Anon., J. AOAC Int. 90(3), 625 (2007)
[2] Biedermann and Grob, J. Chromatogr. A 1255, 56-75 (2012)
[3] Mondello et al., J. Chromatogr. A 1035, 237-247 (2004)
[4] Tamura et al., ASMS Poster TP-739 (2013)
[5] EURL-FV Method 2010-M1; EC Reg. 589/2014; EC Reg. 882/2012