Najam A R, Korver M P, Williams C C, Burse V W, Needham L L
Centers for Disease Control and Prevention, National Center for Environmental Health, Atlanta, GA 30341-3724, USA.
J AOAC Int. 1999 Jan-Feb;82(1):177-85.
An analytical method is presented for precise identification and quantitation of 29 specific polychlorinated biphenyl (PCB) congeners and 15 chlorinated pesticides in human serum. Analyte surrogates PCB 30, PCB 204, 2,2',4,4',5,5'-hexabromo-biphenyl, perthane, alpha-hexachlorocyclohexane, and dichlorobenzophenone were added to each sample. The serum was extracted with an organic solvent and separated by adsorption chromatography into 3 elution fractions for high-resolution gas chromatographic analysis. Each fraction was analyzed by dual-column capillary chromatography followed by electron capture detection. Two capillary columns, DB-5 and DB-1701, with different polarities were used to increase selectivity for each analyte. Quantitation was performed by selecting 2 sets of calibration standard mixtures and 1,2-dichloronaphthalene as an internal standard. Mean recoveries ranged from 39 to 126% for selected analytes and from 31 to 88% for surrogates. Detection limits for specific congeners and pesticides are reported. Typical chromatographic profiles of calibration standard mixtures, as well as a human sample, are illustrated. Verification of each analyte is assessed, and results of analyses of selected human samples and quality control criteria used to ensure data validity also are presented.
本文介绍了一种用于精确鉴定和定量人血清中29种特定多氯联苯（PCB）同系物和15种氯代农药的分析方法。向每个样品中添加分析物替代物PCB 30、PCB 204、2,2',4,4',5,5'-六溴联苯、全氯乙烷、α-六氯环己烷和二氯二苯甲酮。血清用有机溶剂萃取，通过吸附色谱分离为3个洗脱级分，用于高分辨率气相色谱分析。每个级分通过双柱毛细管色谱分析，然后进行电子捕获检测。使用两根极性不同的毛细管柱DB-5和DB-1701来提高对每种分析物的选择性。通过选择2组校准标准混合物并以1,2-二氯萘作为内标进行定量。选定分析物的平均回收率为39%至126%，替代物的平均回收率为31%至88%。报告了特定同系物和农药的检测限。展示了校准标准混合物以及一份人类样品的典型色谱图。评估了每种分析物的验证情况，并给出了选定人类样品的分析结果以及用于确保数据有效性的质量控制标准。
