科研之友
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摘要
The present study considers simple and cost-effective modifications to commercial pressurised solvent extraction cells to extract polychlorinated biphenyls (PCBs) from avian blood and serum. Blood and serum samples of mass 0.2 g were examined. Such masses are consistent with those which may be obtained from many avian species without sacrificing individuals or compromising breeding and (or) migratory success. Extraction vessels are modified by the use of Teflon inserts, which are readily fabricated at low cost. These inserts reduce internal cell volume and surface area. Thus, background contamination is reduced whilst extraction and rinse solvent is used more effectively to afford a small extract volume. Packing of the cell void with sodium sulfate and florisil achieves in situ sample dehydration and lipid removal. When combined with extraction concentration and large volume injection gas chromatography - ion-trap mass spectrometry (LVI-GC-ITMS), the extraction method is capable of polychlorinated biphenyl analysis without post-extraction cleanup. Validation was accomplished using commercial chicken whole blood and serum, and PCB congeners 28, 77, 105, 126, 153, 167, 170, 180, 183, and 194. Surrogate corrected recoveries in the range of 75% to120% for whole blood and 80% to115% for serum were obtained. Detection limits were in the range of 0.01 to 0.22 ng g(-1) for whole blood and 0.03 to 0.45 ng g(-1) for serum. The relative standard deviations for all congeners investigated were better than 15%.
- 出版日期2011-1
