Optimization of detection of twelve polycyclic aromatic hydrocarbons in Carpathian barbel ( Barbus carpathicus ) tissues: extraction methods and GC-MS parameters

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A GC-MS method in selected ion monitoring (SIM) mode was optimized and validated for the determination of twelve polycyclic aromatic hydrocarbons (PAHs) in Barbus carpathicus tissues (muscle and hepatopancreas). Two chromatographic columns (HP-5ms and DB-EUPAH) were evaluated with multiple temperature programs, and the DB-EUPAH column proved superior for separating critical PAH isomers within a 25-minute runtime. Method validation demonstrated excellent linearity (R2 ≥ 0.995), with deviation from linearity <20%, precision expressed as relative standard deviation (RSD ≤ 10%), and detection limits (LOD) ranging from 0.3 to 2.2 ng/mL and quantification limits (LOQ) from 0.95 to 6.85 ng/mL across the twelve validated analytes. Sample preparation optimization comparing ultrasonic and shaker-assisted extraction revealed that mechanical shaker extraction yielded superior results, particularly in the 12–16 min retention time window. Subsequent solid-phase extraction (SPE) purification using dichloromethane as the eluent significantly reduced matrix interference. Overall recovery rates ranged from 63.1% to 146.0%, with eight PAHs meeting acceptable criteria (70–120% recovery) for B.carpathicus tissue analysis. The developed method provides a reliable, validated analytical tool suitable for routine monitoring and risk assessment of PAH contamination in B.carpathicus, supporting environmental monitoring and food safety protocols.

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