GC-MSMS测定中药中18种多氯联苯.PDFVIP

GC-MS/MS 测定中药中 18 种多氯联苯  谭春梅，程巧鸳，马临科，赵维良*(浙江省食品药品检验研究院，杭州 310052) 摘要：目的 建立 GC-MS/MS 测定中药材中 18 种多氯联苯(PCBs)的方法。方法 采用超声提取，浓硫酸净化，内标法 定量；采用EI 源，在多反应监测(MRM)模式下进行检测。结果 18 种 PCBs 在 0.5~50 ng·L1 时线性关系良好，相关系 数(r)为0.999 8~1.000 0 ，方法的检出限为0.013~0.080 μg·kg1 ，定量限为0.054~0.328 μg·kg1。在2 ，5 ，10 μg·L1 下平均 回收率分别为106.7%~118.7%，93.5%~114.7%和89.9%~115.6% ，相对标准偏差分别为1.6%~8.0%，2.7%~4.6%和1.0%~3.1%。 结论 本方法样品处理简单、快速，灵敏度高，准确性好，可用于中药材中18 种PCBs 的测定。 关键词：多氯联苯；气相色谱-三重四级杆质谱联用法；中药材 中图分类号：R917.101 文献标志码：B 文章编号：1007-7693(2017)10-1447-04 DOI: 10.13748/ki.issn1007-7693.2017.10.018 引用本文：谭春梅, 程巧鸳, 马临科, 等. GC-MS/MS 测定中药中18 种多氯联苯[J]. 中国现代应用药学, 2017, 34(10): 1447-1450. Determination of 18 Polychlorinated Biphenyls in Traditional Chinese Medicine with GC-MS/MS * TAN Chunmei, CHEN Qiaoyuan, MA Linke, ZHAO Weiliang (Zhejiang Institute for Food and Drug Control, Hangzhou 310052, China) ABSTRACT: OBJECTIVE To develop a method for the determination of polychlorinated biphenyls (PCBs) in traditional Chinese medicine by GC-MS/MS. METHODS PCBs in traditional Chinese medicine were extracted by ultrasonic and purified by sulfuric acid, internal standard method for quantification; and then determined in multiple reaction monitoring (MRM) mode with EI source. RESULTS The method showed good linearity when the concentration of 18 PCBs were within 0.550.0 ng·L1, with the correlation coefficient (r) within 0.999 81.000 0. The limits of detection were within 0.0130.080 μg·kg1. The limits of quantification were 0.0540.328 μg·kg. The average recoveries were within 106.7 %118.7 % at the spiked levels of 2 μg·L1, within 93.5%114.7% at the spiked levels of 5 μg·L1 and within 89.9 %115.6 % at the spiked levels of 10 μg·L1. The relative standard deriv