凝胶渗透色谱-气相色谱-串联质谱法测定血清中7种多氯联苯残留量

目的:建立了人血清样品中7种多氯联苯残留量的分析方法。方法:样品以丙酮-正己烷(1+2,V/V)为提取溶剂,经高速匀浆方法提取,提取液经凝胶渗透色谱净化,除去样品中大部分的血糖和蛋白等干扰基质,采用VF-5ms(30 m×0.25 mm×0.25μm)色谱柱对7种多氯联苯进行分离,通过多反应离子监测模式扫描检测,有效地降低了样品中的复杂基质所带来的背景干扰。采用色谱保留时间和质谱碎片离子丰度比定性,外标法定量。结果:方法的相关系数r>0.999,最小检出限为0.5μg/kg～1.0μg/kg。在3种浓度添加水平5.0μg/kg、10.0μg/kg、20.0μg/kg下,其平均回收率为87.6%～101%,相对标准偏差为2.5%～10.3%(n=6)。结论:实验证明,该方法是一种快速、准确、灵敏度高的检测血清样品中多氯联苯残留量的检测方法。

Determination of 7 kinds of polychlorinated biphenyls residues in Human serum using gel permeation chromatography and Gas Chromatography-Mass/Mass spectrum

Objective: To develop an analytical method for determination of 7 PCBs in human serum.Methods: With acetone-hexane(1+2,V/V) as the extraction solution,the samples were extracted by means of high-speed homogenization.And the crude extract was purified by GPC extraction column to remove most blood sugar and protein in samples.The 7 PCBs were separated by VF-5(30 m×0.25 mm×0.25 μm)column and the background interference brought about by the complex matrix in samples was effectively reduced.The PCBs were qualitatively and quantitatively determined under multi-reaction monitoring(MRM) scan type with tandem mass analyzer.Results:The method could be used to determine the PCBs residue in sample with fine linear relationship(r>0.999).The limits of detection(LOD) were 0.5 μg/kg～1.0 μg/kg.At the spiked levels of 5.0,10.0 and 20.0 μg/kg,the mean recoveries were in the range of 87.6% to 101%,and the relative standard deviations(RSDs) were in the range of 2.5% to 10.3%(n=6).Conclusion:Experiments showed that the method was rapid,accurate and highly senstive,which can be used for the detemination of PCBs residues in human serum.