| 引用本文: | 谭春梅,程巧鸳,马临科,赵维良.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. |
| TAN Chunmei,CHEN Qiaoyuan,MA Linke,ZHAO Weiliang.Determination of 18 Polychlorinated Biphenyls in Traditional Chinese Medicine with GC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2017,34(10):1447-1450. |
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| 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 |
| DOI：10.13748/j.cnki.issn1007-7693.2017.10.018 |
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| Determination of 18 Polychlorinated Biphenyls in Traditional Chinese Medicine with GC-MS/MS |
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TAN Chunmei, CHEN Qiaoyuan, MA Linke, ZHAO Weiliang
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Zhejiang Institute for Food and Drug Control, Hangzhou 310052, China
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| 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. |
| Key words: polychlorinated biphenyls Gas chromatography triple quadrupole mass spectrometry traditional Chinese medicine |
