Determination of indicator polychlorinated biphenyls in vegetable oils by double clean-up-gas chromatography

doi:10.3724/SP.J.1123.2014.06010

Abstract

Abstract:

To investigate the residues of seven indicator polychlorinated biphenyls (PCBs) in vegetable oils, a method was established for the determination of trace PCBs in vegetable oils by double clean-up coupled with gas chromatography (GC). After extracted with acetonitrile, the sample extract was concentrated to dryness followed by re-dissolving with hexane. And the solution was pretreated by adding concentrated sulfuric acid followed cleaned-up with silica gel in dispersive solid-phase extraction protocol, then analyzed by GC with external standard method. Under the optimized chromatographic conditions, the analysis was carried out with a capillary column (HP-5, 30 m×0.32 mm×0.25 μm) at a flow rate of 0.8 mL/min, and the sample volume was 1.00 μL. Monitoring with an electron-capture detector, all the target analytes were separated by temperature-programming of the column. Good linearities were obtained in the range of 10-500 μg/L for the seven indicator PCBs with the correlation coefficients greater than 0.999. For different matrices, the limits of detection (S/N=3) and limits of quantitation (S/N=10) were in the range of 1.8-8.9 μg/kg and 5.9-29.8 μg/kg, respectively. At three spiked levels of 10, 20 and 100 μg/kg of the seven indicator PCBs in olive oil, palm oil and peanut oil blank samples, the average recoveries ranged from 71.0% to 105.5% with the RSDs of 4.0%-11.3%. The method is simple, rapid and accurate, and can be used for the routine analysis of the indicator PCBs in vegetable oils.

Key words: double clean-up, gas chromatography (GC), polychlorinated biphenyls (PCBs), residues, vegetable oils

CLC Number:

O658

DING Liping, CAI Chunping, WANG Danhong. Determination of indicator polychlorinated biphenyls in vegetable oils by double clean-up-gas chromatography[J]. Chinese Journal of Chromatography, 2014, 32(11): 1266-1270.

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