摘要
目的建立UPLC-MS/MS同时测定复方胃痛胶囊中马兜铃酸Ⅰ和马兜铃酸Ⅱ含量的方法。方法采用Agilent Poroshell SB-C18色谱柱(100 mm×2.1 mm,2.7μm);流动相为乙腈和含5 mmol/L甲酸铵的0.1%甲酸溶液,梯度洗脱,流速为0.3 mL/min,柱温为30℃;采用三重四级杆质谱检测器,电喷雾离子源(ESI)正离子模式下多反应监测(MRM)模式进行质谱检测。结果马兜铃酸Ⅰ和马兜铃酸Ⅱ分别在1.05~210 ng/mL(r=0.9996)和1.00~200 ng/mL(r=0.9998)有良好的线性关系。马兜铃酸Ⅰ的回收率为95.90%,RSD为2.11%;马兜铃酸Ⅱ的回收率为93.22%,RSD为1.17%。马兜铃酸Ⅰ的定量限为0.3 pg、检出限为0.1 pg;马兜铃酸Ⅱ的定量限为0.7 pg、检出限为0.2 pg。结论该方法专属性好,灵敏度高,准确可靠,能够用于测定复方胃痛胶囊中马兜铃酸Ⅰ和马兜铃酸Ⅱ的含量。
Objective To establish an UPLC-MS/MS method for simultaneous determination of aristolochic acid I and aristolochic acid II in fufang weitong capsules.Methods Agilent Poroshell SB-C18(100 mm×2.1 mm,2.7μm)column was used for separation.The mobile phase consisted of acetonitrile and 0.1%formic acid(containing 5 mmol/L ammonium formate)with gradient elution.The flow rate was 0.3 mL/min and the column temperature was 30℃.Electrospray positive ion source was used for mass spectrometry detection by multiple reaction monitoring mode.Results The liner range of calibration curve was 1.05-210 ng/mL(r=0.9996),1.00-200 ng/mL(r=0.9999)for aristolochic acid I and aristolochic acid II.The recovery of aristolochic acidⅠwas 95.90%with RSD of 2.11%,and the recovery of aristolochic acidⅡwas 93.22%with RSD of 1.17%.The limit of detection and quantitation for aristolochic acid I were 0.3 pg and 0.1 pg,for aristolochic acid II were 0.7 pg and 0.2 pg.Conclusion The method has good specificity,sensitivity and accuracy,and it is suitable for the content determination of aristolochic acid I and aristolochic acid II in fufang weitong capsules.
作者
彭玲娜
梁晟
孙辉
丁野
李文莉
刘静
戴忠
马双成
PENG Lingna;LIANG Sheng;SUN Hui;DING Ye;LI Wenli;LIU Jing;DAI Zhong;MA Shuangcheng(Hunan Institute of Drug Inspection and Testing,Hunan Engineering and Technology Research Center for Pharmaceutical Quality Evaluation,Changsha Hunan 410001,China;National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《药品评价》
CAS
2024年第1期15-19,共5页
Drug Evaluation
基金
2022年度国家药品标准制修订研究课题(2021Z15-2)。
