Development and validation of a gas chromatography method for analysing polychlorinated biphenyls in fish roe

Abstract

A method for determining polychlorinated biphenyls (PCBs) in fish roe by gas chromatography (GC) has been developed. The suitability (validation) of the process for the determination of 14 PCBs (PCB 18, PCB 31, PCB 28, PCB 52, PCB 44, PCB 101, PCB 149, PCB 118, PCB 153, PCB 138, PCB 180, PCB 170, PCB 194, PCB 209) in fish roe by GC using an electron capture detector (ECD) was evaluated according to the following criteria: selectivity, linearity, limits of detection (LOD), limits of quantification (LOQ), accuracy and precision. Automated Soxhlet extraction and sample clean-up by solid phase extraction (SPE) were proposed for extracting PCBs from fish roe. The results of the method selectivity study showed that the determination of PCBs in fish roe is not affected by other components in the sample. The correlation coefficients for fourteen PCBs ranged from 0.9962 to 0.9999 (R2 ≥0.995). The limits of detection (LOD) and limits of quantification (LOQ) of PCBs are below the maximum permissible levels set by the European Union (EU). The recovery percentage ranged from 81.5% to 107%, indicating the PCB extraction procedure's acceptability (R, 80 – 120%). The relative standard deviation (RSD, %) of the measurement results under convergence conditions ranged from 1.02% to 9.43% (RSD ≥15%). The obtained method suitability (validation) data meets the Commission Regulation (EU) No 589/2014 criteria.

Keywords

• fish roe
• polychlorinated biphenyls
• PCB
• gas chromatography
• GC
• method validation