首页|超高效液相色谱串联质谱法测定复方胃痛胶囊中马兜铃酸Ⅰ、马兜铃酸Ⅱ的含量

超高效液相色谱串联质谱法测定复方胃痛胶囊中马兜铃酸Ⅰ、马兜铃酸Ⅱ的含量

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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。7 μm);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。999 6)和 1。00~200 ng/mL(r=0。999 8)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。
Content Determination of Aristolochic Acid Ⅰ and Aristolochic Acid Ⅱ in Fufang Weitong Capsules by UPLC-MS/MS
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,2.7 µm)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=0.999 6),1.00-200 ng/Ml(r=0.999 9)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 acid Ⅱ was 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.

Fufang weitong capsulesAristolochic acid analogsUPLC-MS/MS

彭玲娜、梁晟、孙辉、丁野、李文莉、刘静、戴忠、马双成

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湖南省药品检验检测研究院,湖南省药品质量评价工程技术中心,湖南 长沙 410001

中国食品药品检定研究院,北京 100050

复方胃痛胶囊 马兜铃酸 超高效液相色谱串联质谱法

2022年度国家药品标准制修订研究课题

2021Z15-2

2024

药品评价
江西省药学会

药品评价

影响因子:0.672
ISSN:1672-2809
年,卷(期):2024.21(1)
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