HPLC, GCxGC, GC/MSD, GC/TOF
IndustriesFood & Agriculture
ManufacturerLECO, Restek
Importance of the Topic
Mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) are petroleum-derived contaminants found in food through packaging and processing. MOSH can accumulate in human tissues, while MOAH may exhibit genotoxicity, prompting regulatory bodies like EFSA to request comprehensive data on oil-derived impurities.
Objectives and Study Overview
This study addresses EFSA’s data gap by developing an analytical workflow for simultaneous MOSH, MOAH, and PAH screening in food additives and matrices, using combined HPLC fractionation with GC×GC-FID and high-resolution TOFMS.
Methodology and Instrumentation Used
The analytical procedure comprises:
- Sample extraction from food or additives, followed by HPLC purification to isolate MOSH, MOAH, and remove coeluting interferences.
- GC×GC separation: first dimension on a 10 m × 0.53 mm Rxi-17Sil MS column; second dimension on an 0.8 m × 0.15 mm Rxi-1MS column with cryogenic modulation.
- Detection: FID for quantitative measurement of hydrocarbon “humps” with uniform response; TOFMS for structural characterization, identification of contamination markers, and selective PAH quantitation.
Main Results and Discussion
The combined HPLC/GC×GC-FID/TOFMS system demonstrates:
- Enhanced resolution of MOSH and MOAH fractions and effective removal of interferences through HPLC.
- Structured 2D chromatograms enabling classification of MOAH by aromatic ring count (1–2 vs. ≥3 rings).
- Detection of source-specific markers (e.g., DIPN indicating recycled paperboard migration) via characteristic GC×GC patterns and MS signals.
- Simultaneous quantitation: MOSH/MOAH at 0.5–1 mg/kg as quantitative humps and PAHs at 0.9 µg/kg as discrete peaks.
- High PAH recovery using HPLC purification without epoxidation, simplifying PAH analysis.
Benefits and Practical Applications
This advanced platform surpasses routine HPLC-GC-FID by providing structural insights, interference-free quantitation, contamination source attribution, and multi-class contaminant screening for regulatory compliance and QA/QC in food safety laboratories.
Future Trends and Opportunities
Emerging directions include:
- Automated HPLC-GC×GC workflows for high-throughput screening.
- Profiling of novel hydrocarbon contaminants in diverse food matrices.
- Chemometric integration for pattern recognition and source tracking.
- On-line coupling with complementary detectors (e.g., NMR) for deeper molecular elucidation.
Conclusion
The HPLC/GC×GC-FID/TOFMS approach offers a versatile, high-resolution platform for comprehensive MOSH, MOAH, and PAH analysis, fulfilling EFSA recommendations and advancing food safety monitoring through combined sensitivity, selectivity, and structural clarity.
Used Instrumentation
- High-performance liquid chromatography (HPLC) for fractionation and purification.
- Comprehensive two-dimensional gas chromatography (GC×GC) with cryogenic modulation.
- Flame ionization detector (FID) for uniform quantitative hydrocarbon response.
- Time-of-flight mass spectrometer (TOFMS) for high-resolution mass spectra and contaminant identification.
References
- Gorska A., Bellinghieri C., Albendea P., Purcaro G. (2025) Application of HPLC/GC×GC-FID/TOFMS for MOSH/MOAH analysis in food ingredients. Analytical Chemistry – Gembloux Agro-Bio Tech.
- Biedermann M., Grob K. (2015) Identification of DIPN as a marker for mineral oil migration from recycled paperboard. Journal of Chromatography A 1375, 146–153.
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