UPLC-MS/MS测定追风透骨丸中马兜铃酸类成分含量  

Determination of Aristolochic Acids and Their Derivates in Zhuifeng Tougu Pills by UPLC-MS/MS

作　　者：王颖 刘繁红 杨燕丽 何筱毅 何成军 杨蕾 袁军 戴忠[2] WANG Ying;LIU Fan-hong;YANG Yan-li;HE Xiao-yi;HE Cheng-jun;YANG Lei;YUAN Jun;DAI Zhong(National Medical Products Administration Key Laboratory of Quality Evaluation of Chinese Patent Medicines,Sichuan Institute for Drug Control,Chengdu 610097,China;National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]四川省药品检验研究院国家药品监督管理局中成药质量评价重点实验室,四川成都610097 [2]中国食品药品检定研究院,北京100050

出　　处：《中国现代中药》2023年第10期2207-2212,共6页Modern Chinese Medicine

基　　金：国家药典委员会2021年度国家药品标准制修订研究课题(2021Z16)。

摘　　要：目的:建立超高效液相色谱-质谱法(UPLC-MS/MS)同时测定追风透骨丸中马兜铃酸Ⅰ、马兜铃酸Ⅱ、马兜铃酸Ⅲ和马兜铃内酰胺Ⅰ的含量。方法:采用Waters ACQUITY UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8μm);以乙腈-0.1%甲酸水溶液(含5 mmol·L^(-1)甲酸铵)为流动相梯度洗脱,流速为0.3 mL·min^(-1),用电喷雾离子源,在多反应监测模式下采用外标法测定。结果:4个成分在2~250 ng·mL^(-1)线性关系良好,r均大于0.999,在20 ng·mL^(-1)添加水平的平均回收率分别为104.2%、75.7%、112.0%、105.4%,RSD为2.8%~6.1%,方法定量限为0.002~0.100μg·g^(-1)。7批样品中均未检出马兜铃酸Ⅱ、马兜铃酸Ⅲ,马兜铃酸Ⅰ检出量为0.09~0.41μg·g^(-1),马兜铃内酰胺Ⅰ检出量为0.62~1.30μg·g^(-1)。结论:该方法专属性好、灵敏度高、结果准确,可为追风透骨丸中马兜铃酸的质量控制提供参考。Objective:To establish a method for determining the aristolochic acids and their derivates in Zhuifeng Tougu Pills by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods:The gradient elution was carried out in the Waters ACQUITY UPLC HSS T3 column(100 mm×2.1 mm,1.8μm)with acetonitrile-0.1%formic acid(containing 5 mmol·L^(-1) ammonium formate)as the mobile phase at a flow rate of 0.3 mL·min^(-1).Under electrospray ionization and multiple reaction monitoring(MRM)mode,the content was determined with the external standard method.Results:The 4 components showed a good linear relationship within 2-250 ng·mL^(-1)(r>0.999).The average recovery of the 4 components was 104.2%,75.7%,112.0%,and 105.4%,respectively,at the addition amount of 20 ng·mL^(-1),and the relative standard deviations(RSDs)varied within the range of 1.9%-6.1%.The limits of quantitation(LOQs)were 0.002-0.100μg·g^(-1).Aristolochic acidsⅡandⅢwere detected in none of the 7 batches of samples.The content of aristolochic acidⅠand aristolactamⅠin the samples was in the range of 0.09-0.41μg·g^(-1) and 0.62-1.30μg·g^(-1),respectively.Conclusion:The method is simple,sensitive,and reliable and can be applied to determination of aristolochic acid analogues in Zhuifeng Tougu Pills.

关 键 词：液相色谱-质谱法 多反应监测 马兜铃酸Ⅰ 马兜铃酸Ⅱ 马兜铃酸Ⅲ 马兜铃内酰胺Ⅰ 追风透骨丸 

分 类 号：R286[医药卫生—中药学]