Determination and validation of polycyclic aromatic hydrocarbons (PAH4) in katsuobushi, plant-based food supplements, and cocoa bean shells using GC-MS/MS.

Polycyclic aromatic hydrocarbons (PAHs) are primarily generated through the incomplete combustion or pyrolysis of organic materials in various industrial processes. Foods may become contaminated with environmental PAHs found in air, soil, or water, or through industrial food processing methods such as smoking, roasting, drying, and grilling. The Ministry of Health and Welfare in Taiwan has established maximum levels for benzo[a]pyrene (BaP) and indicative values for BaP as well as PAH4 (the sum of benz[a]anthracene, chrysene, benzo[b]fluoranthene, and benzo[a]pyrene) in foods as operational guidelines. The current study developed an analytical method for simultaneous determination of PAH4 levels in katsuobushi (dried bonito flakes), cocoa bean shells, and plant-based food supplements using gas chromatography-tandem mass spectrometry (GC-MS/MS). Sample preparation methods were assessed using cyclohexane extraction and solid-phase extraction (SPE) for purification. PAH4 levels were subsequently quantified with matrix-matched calibration curves combined with isotopic internal standards. The limit of quantitation (LOQ) for each PAH was 5 μg/kg for katsuobushi and plant-based food supplements, and 1 μg/kg for cocoa bean shells. The effectiveness of the method was validated through each PAH analyte in the matrices of katsuobushi, cocoa bean shells, and plant-based food supplements. The average recoveries of PAH4 for fortified samples in each matrix ranged from 101.1 to 115.6% with all coefficients of variation being less than 6.5%. This method is applicable for routine analysis of PAH4 in a diverse array of food products to ensure food safety.