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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 establish a method for the determination of 18 polychlorinated biphenyls (PCBs) in Chinese herbal medicines by GC-MS / MS. Methods Ultrasound extraction, concentrated sulfuric acid purification and internal standard method were used for quantification. EI sources were used for detection in multiple reaction monitoring (MRM) mode. Results The linearity of 18 PCBs was good at 0.5 ~ 50 ng · L ~ (-1), the correlation coefficient (r) was 0.999 8 ~ 1.000 0, and the detection limit was 0.013 ~ 0.080 μg · kg ~ (-1) , The limit of quantification was 0.054 ~ 0.328μg · kg ~ (-1). The average recoveries were 106.7% -118.7%, 93.5% -114.7% and 89.9% -115.6% at 2, 5 and 10μg · L -1, respectively. The relative standard deviations were 1.6% -8.0%, 2.7% ~ 4.6% and 1.0% ~ 3.1%. Conclusion The method is simple, rapid, sensitive and accurate. It can be used for the determination of 18 kinds of PCBs in Chinese herbal medicines.