摘要
目的:建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定5种马兜铃属药材中马兜铃酸A、B、C、D含量的方法。方法:采用Agilent Zorbax Extend C18色谱柱(2. 1 mm×100 mm,1. 8μm),电喷雾离子源,多反应监测(MRM)模式,正离子检测,定量离子对为马兜铃酸A:m/z359. 1→298. 1;马兜铃酸B:m/z 329. 0→268. 0;马兜铃酸C:m/z 345. 2→282. 0;马兜铃酸D:m/z 375. 0→212. 0;内标金合欢素:m/z 285. 0→242. 0。结果:马兜铃酸A在0. 06～12μg/mL范围内呈现良好的线性关系(r=0. 9967);马兜铃酸B在0. 055～11μg/mL范围内呈现良好的线性关系(r=0. 9980);马兜铃酸C在0. 065～13μg/mL (r=0. 9969)范围内呈现良好的线性关系;马兜铃酸D在0. 06～12μg/mL (r=0. 9982)范围内呈现良好的线性关系。马兜铃酸A、B、C、D平均加样回率分别为89. 95%、92. 06%、91. 06%、92. 18%,RSD分别为3. 88%、3. 97%、4. 79%、4. 76%。结论:该方法快速、灵敏度高、专属性好,可作为马兜铃属药材的一种质量控制评价方法。
Objective To establish a UPLC-MS/MS method for determination of Aristolochic acid A、B、C、D in five Aristolochia herbs by UPLC-MS/MS. Methods Chromatographic analysis was conducted on a Agilent Zorbax Extend C_（18） column（ 2. 1 mm ×100 mm,1. 8 μm）. Detection and quantification were performed by mass spectrometry in multiple reaction monitoring（ MRM） mode with m/z 359. 1→298. 1 for aristolochic acid A; m/z 329. 0→268. 0 for aristolochic acid B; m/z 345. 2→282. 0 for aristolochic acid C; m/z 375. 0→212. 0 for aristolochic acid D; and m/z 285. 0→242. 0 for acacetin（ internal standard）. Results Aristolochic acid A showed good linear relationships within the range of 0. 06 ～ 12 μg·mL^（-1）（ r = 0. 9967）; Aristolochic acid B showed good linear relationships within the range of 0. 055 ～ 11 μg·mL^（-1）（ r = 0. 9980）; Aristolochic acid C showed good linear relationships within the range of 0. 065 ～ 13 μg·mL^（-1）（ r = 0. 9969）; Aristolochic acid D showed good linear relationships within the range of 0. 06 ～ 12 μg·mL^（-1）（ r = 0. 9982）. The average recoveries were 89. 95% 、92. 06% 、91. 06% 、92. 18%,respectively,the relative standard deviations（ RSD） were 3. 88% 、3. 97% 、4. 79% 、4. 76%,respectively. Conclusion The proposed method is rapid,sensitive,specific,which could be an effective method for the quality control of Aristolochia herbs
作者
丁慧
沈君子
费文静
钱勇
谢天培
刘倩
DING Hui;SHEN Junzi;FEI Wenjing;QIAN Yong;XIE Tianpei;LIU Qian(Standard Testing Lab（Shanghai）Co.,Ltd.,Shanghai 201203,China)
出处
《中国民族民间医药》
2018年第18期38-43,共6页
Chinese Journal of Ethnomedicine and Ethnopharmacy
基金
上海市科研计划项目(15DZ0503300)
