UPLC-MS/MS法同时测定小活络丸中3种功效成分和3种毒性成分  

Simultaneous determination of three effective constituents and three toxic constituents in Xiaohuoluo Pills

作　　者：钱岩 顾臣贤 吴杨 王天宇 李华露 闵春艳 QIAN Yan;GU Chen-xian;WU Yang;WANG Tian-yu;LI Hua-lu;MIN Chun-yan(Suzhou Institute for Drug Control,Suzhou 215104,China;Soochow University,Suzhou 215006,China;Nanjing University of Traditional Chinese Medicine,Nanjing 210046,China)

机构地区：[1]苏州市药品检验检测研究中心,江苏苏州215104 [2]苏州大学,江苏苏州215006 [3]南京中医药大学,江苏南京210046

出　　处：《中成药》2022年第10期3120-3125,共6页Chinese Traditional Patent Medicine

基　　金：江苏省药品监督管理局科研项目(20170214)。

摘　　要：目的 建立超高效液相色谱-三重四级杆串联质谱(UPLC-MS/MS)法同时测定小活络丸(胆南星、制川乌、制草乌等)中功效成分(苯甲酰乌头原碱、苯甲酰次乌头原碱、苯甲酰新乌头原碱)、毒性成分(乌头碱、次乌头碱、新乌头碱)的含量。方法 该药物甲醇提取液的分析采用Waters Acquity BEH C_(18)色谱柱(2.1 mm×50 mm, 1.7μm);流动相乙腈-0.1%甲酸,梯度洗脱;体积流量0.4 mL/min;柱温30℃;电喷雾离子源,正离子检测,多反应监测模式。结果 6种成分在各自范围内线性关系良好(r≥0.995 6),平均加样回收率98.33%~102.14%,RSD 2.98%~7.88%。14批样品中功效成分、毒性成分含量集中,表现出较好的质量均一性;2批样品中功效成分总含量超过限度范围;所有16批样品中毒性成分总含量均符合相关规定。结论 该方法稳定可靠,可用于小活络丸的质量控制。AIM To establish a ultra performance liquid chromatography-tandem quadrupole mass spectrometry(UPLC-MS/MS) method for the simultaneous content determination of effective constituents(benzoylaconine, benzoylhypaconine, benzoylmesaconine) toxic constituents(aconitine, hypaconitine, mesaconitine) in Xiaohuoluo Pills(Arisaema cum Bile, Aconiti Radix Cocta, Aconiti kusnezoffii Radix Cocta, etc.METHODS The analysis of methanol extract of this drug was performed on a 30 ℃ thermostatic Waters Acquity BEH C_(18) column(4.6 mm×250 mm, 5 μm), with the mobile phase comprising of acetonitrile-0.1% formic acid flowing at 0.4 mL/min in a gradient elution manner, and electron spray ionization source was adopted in positive ion detection with multiple reaction monitoring mode.RESULTS Six constituents showed good linear relationships within their own ranges(r≥0.995 6), whose average recoveries were 98.33%-102.14% with the RSDs of 2.98%-7.88%. The contents of effective constituents and toxic constituents were concentrative in fourteen batches of samples, demonstrating good quality uniformity. The total contents of effective constituents in two batches of samples exceeded limit ranges, and those of toxic constituents in all the sixteen batches of samples accorded with related requirements.CONCLUSION This sTab.and reliable method can be used for the quality control of Xiaohuoluo Pills.

关 键 词：小活络丸 功效成分 毒性成分 超高效液相色谱-三重四级杆串联质谱(UPLC-MS/MS) 

分 类 号：R927.2[医药卫生—药学]