Analysis of Polycyclic Aromatic Hydrocarbons (PAHs) in Foods by GC-MS/MS

Význam tématu

Polycyclic aromatic hydrocarbons (PAHs) are persistent environmental pollutants generated during incomplete combustion processes. They commonly contaminate smoked and dried foods, raising health concerns due to their mutagenic and carcinogenic properties. Regulatory bodies worldwide have established maximum limits for key PAHs such as benzo[a]pyrene to protect consumer safety. Accurate, sensitive, and reliable analytical methods are therefore essential for routine monitoring and compliance.

Cíle a přehled studie

This study aimed to develop and validate a gas chromatography–tandem mass spectrometry (GC-MS/MS) method for the quantification of 16 priority PAHs in katsuobushi (dried, smoked, and fermented skipjack tuna). The objectives included optimizing chromatographic separation, minimizing detection limits, and demonstrating improved performance compared to conventional GC-MS in selected ion monitoring (SIM) mode.

Použitá metodika a instrumentace

Sample Preparation and Extraction:

• Katsuobushi samples underwent solvent extraction and cleanup prior to injection.

Instrumentation:

• GC-MS/MS system: Shimadzu GCMS-TQ8040
• Column: RESTEK Rxi-PAH, 60 m × 0.25 mm I.D., 0.1 µm film thickness
• Injection: Splitless, 2 µL, inlet temperature 330 °C
• Carrier gas: Helium at constant linear velocity (40 cm/s)
• Oven program: 180 °C (2 min) ramp to 260 °C at 5 °C/min, then to 350 °C at 15 °C/min (12 min)
• MS/MS conditions: Interface 330 °C, ion source 230 °C, multiple reaction monitoring (MRM), loop time 0.3 s

Hlavní výsledky a diskuse

Detection Limits:

• MRM mode achieved lower or comparable limits of detection (0.011–0.134 pg/µL) for all target PAHs versus SIM mode (0.017–0.323 pg/µL).

Chromatographic Performance:

• MRM provided sharper peaks and clearer baseline separation, improving identification in complex katsuobushi extracts.
• Comparison of SIM and MRM chromatograms for benzo[a]pyrene and indeno[1,2,3-cd]pyrene demonstrated enhanced signal-to-noise ratio in MS/MS.

Discussion:

• The highly selective MRM transitions reduced interferences and elevated sensitivity, facilitating reliable quantification at trace levels.

Přínosy a praktické využití metody

The GC-MS/MS approach offers robust, high-throughput analysis for food safety laboratories and QA/QC operations. Key benefits include:

• Lower detection limits enabling compliance with stringent regulatory thresholds.
• Improved selectivity in complex matrices such as smoked fish products.
• Automated MRM setup via Smart MRM software, reducing method development time.

Budoucí trendy a možnosti využití

Advances likely include integration of faster GC temperature programming, miniaturized sample preparation, and high-resolution MS detectors to further lower detection limits. Expansion to other food matrices and environmental samples will broaden applications. Coupling with data analytics and automated workflows may enhance throughput and regulatory reporting.

Závěr

This application demonstrates that GC-MS/MS in MRM mode significantly outperforms traditional SIM-based GC-MS for PAH analysis in katsuobushi. The method delivers superior sensitivity, selectivity, and reproducibility, making it well suited for routine monitoring of carcinogenic contaminants in food.

Reference

• Shimadzu Corporation. Analysis of Polycyclic Aromatic Hydrocarbons in Foods by GC-MS/MS. Application Data Sheet LAAN-J-MS-E109. First Edition April 2015.