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

关键词:  多氯联苯  气相色谱-三重四级杆质谱联用法  中药材

Key words:  polychlorinated biphenyls  Gas chromatography triple quadrupole mass spectrometry  traditional Chinese medicine

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。

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^-1. 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 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.