UPLC-MS/MS测定追风透骨丸中马兜铃酸类成分含量OACSTPCD
Determination of Aristolochic Acids and Their Derivates in Zhuifeng Tougu Pills by UPLC-MS/MS
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,1.8 μm);以乙腈-0.1%甲酸水溶液(含5 mmo·l 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 0.002～0.100 μg·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 0.09～0.41 μg·g-1,马兜铃内酰胺Ⅰ检出量为 0.62～1.30 μg·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,1.8 μm)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 0.002-0.100 μg·g-1.Aristolochic acids Ⅱ and Ⅲ were detected in none of the 7 batches of samples.The content of aristolochic acid Ⅰ and aristolactam Ⅰ in the samples was in the range of 0.09-0.41 μg·g-1 and 0.62-1.30 μg·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.
王颖;刘繁红;杨燕丽;何筱毅;何成军;杨蕾;袁军;戴忠
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中国食品药品检定研究院,北京 100050
中医学
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
UPLC-MS/MSMRMaristolochic acid Ⅰaristolochic acid Ⅱaristolochic acid Ⅲaristolactam ⅠZhuifeng Tougu Pills
《中国现代中药》 2023 (10)
2207-2212,6
国家药典委员会2021年度国家药品标准制修订研究课题(2021Z16)
评论