论文部分内容阅读
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。
OBJECTIVE: To establish an analytical method for the determination of 7 PCBs in human serum samples. Methods: The sample was extracted with acetone-n-hexane (1 + 2, V / V) and extracted by high speed homogenization. The extract was purified by gel permeation chromatography to remove most of the interference matrix such as blood glucose and protein, Seven polychlorinated biphenyls (PCBs) were separated on a VF-5ms (30 m × 0.25 mm × 0.25 μm) column and detected by multiple reactive ion monitoring mode, effectively reducing the background interference caused by the complex matrix in the sample . Chromatographic retention time and mass spectral fragment ion abundance than qualitative, external standard method. Results: The correlation coefficient of the method was more than 0.999, and the minimum detection limit was 0.5μg / kg ~ 1.0μg / kg. The average recoveries were 87.6% ~ 101% and the relative standard deviations (RSDs) were 2.5% ~ 10.3% (n = 6) at the concentration of 5.0μg / kg, 10.0μg / kg and 20.0μg / kg. Conclusion: The experiment proved that this method is a rapid, accurate and sensitive method for the determination of PCBs in serum samples.