GC-MS/MS测定中药中18种多氯联苯

Determination of 18 Polychlorinated Biphenyls in Traditional Chinese Medicine with GC-MS/MS

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0.013~0.080μg·kg^(-1),定量限为0.054~0.328μg·kg^(-1)。在2,5,10μg·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。

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 E1 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 ~tg.kg-1. The limits of quantification were 0.054-0.328μg·kg-1. The average recoveries were within 106.7 %-118.7 % at the spiked levels of 2μg·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 derivations were within 1.6%-8.0%, 2.7%-4.6% and 1.0%-3.1%, respectively. CONCLUSION The method for determination of PCBs in traditional Chinese medicine was rapid, simple, sensitive and accurate. It is suitable for determination of 18 PCBs in traditional Chinese medicine.