中国现代中药2024,Vol.26Issue(8) :1294-1299.DOI:10.13313/j.issn.1673-4890.20240417001

UPLC-MS/MS测定双辛鼻窦炎颗粒中马兜铃酸Ⅰ和马兜铃酸Ⅱ的含量

Determination of Aristolochic Acid Ⅰ and Aristolochic Acid Ⅱ in Shuangxin Bidouyan Granules by UPLC-MS/MS

郭日新 肖萌 刘静 戴忠 魏锋
中国现代中药2024,Vol.26Issue(8) :1294-1299.DOI:10.13313/j.issn.1673-4890.20240417001

UPLC-MS/MS测定双辛鼻窦炎颗粒中马兜铃酸Ⅰ和马兜铃酸Ⅱ的含量

Determination of Aristolochic Acid Ⅰ and Aristolochic Acid Ⅱ in Shuangxin Bidouyan Granules by UPLC-MS/MS

郭日新 1肖萌 1刘静 1戴忠 1魏锋1
扫码查看

作者信息

  • 1. 中国食品药品检定研究院,北京 100050
  • 折叠

摘要

目的:同时测定双辛鼻窦炎颗粒中马兜铃酸Ⅰ和马兜铃酸Ⅱ的含量,为其质量控制提供参考.方法:采用超高效液相色谱-质谱法(UPLC-MS/MS)同时测定双辛鼻窦炎颗粒中马兜铃酸Ⅰ和马兜铃酸Ⅱ的含量.采用 Waters ACQUITY UPLC HSS T3 色谱柱(100 mm×2.1 mm,1.8 μm),乙腈(A)-0.1%甲酸水溶液(含 1 mmol·L-1 乙酸铵,B)为流动相梯度洗脱,电喷雾离子源,正离子扫描,多反应监测模式,以标准曲线法计算样品中马兜铃酸Ⅰ和马兜铃酸Ⅱ的含量.结果:12 批双辛鼻窦炎颗粒中 9 批样品未检出马兜铃酸Ⅰ(检出限0.13 pg),3 批样品检出马兜铃酸Ⅰ,质量分数为 14.62~25.82 ng·g-1.所有样品均未检出马兜铃酸Ⅱ(检出限0.44 pg).结论:建立的UPLC-MS/MS同时测定双辛鼻窦炎颗粒中马兜铃酸Ⅰ和马兜铃酸Ⅱ含量的方法,专属性强、灵敏度高、重复性好,可为双辛鼻窦炎颗粒中马兜铃酸Ⅰ和马兜铃酸Ⅱ的质量控制提供参考.

Abstract

Objective:To simultaneously determine the content of aristolochic acid Ⅰ and aristolochic acid Ⅱ in Shuangxin Bidouyan Granules,and provide a reference for their quality control.Methods:Ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was used to simultaneously determine the content of aristolochic acid Ⅰ and aristolochic acid Ⅱ in Shuangxin Bidouyan Granules.A Waters ACQUITY UPLC HSS T3 column(100 mm×2.1 mm,1.8 μm)was used with a gradient elution of acetonitrile(A)and 0.1%formic acid in water(containing 1 mmol·L-1 ammonium acetate,B)as the mobile phase.An electrospray ionization(ESI)source in positive ion multiple reaction monitoring mode was employed.The content of aristolochic acid Ⅰ and aristolochic acid Ⅱ in the samples were calculated using the standard curve method.Results:Among 12 batches of Shuangxin Bidouyan Granules,aristolochic acidⅠ was not detected in 9 batches(detection limit 0.13 pg),while it was detected in 3 batches with a mass fraction ranging from 14.62 to 25.82 ng·g-1.Aristolochic acid Ⅱ was not detected in any of the samples(detection limit 0.44 pg).Conclusion:The established UPLC-MS/MS method for the simultaneous determination of aristolochic acid Ⅰ and aristolochic acid Ⅱ in Shuangxin Bidouyan Granules is highly specific,sensitive,and reproducible.This method provides a reference for the quality control of aristolochic acid Ⅰ and aristolochic acid Ⅱ in Shuangxin Bidouyan Granules.

关键词

双辛鼻窦炎颗粒/马兜铃酸Ⅰ/马兜铃酸Ⅱ/超高效液相色谱-质谱法/含量测定

Key words

Shuangxin Bidouyan Granules/aristolochic acid Ⅰ/aristolochic acid Ⅱ/UPLC-MS/MS/content determine

引用本文复制引用

基金项目

国家药品监督管理局药品监管科学体系建设重点项目(RS2024Z006)

中国食品药品检定研究院关键技术研究子课题(GJJS-2022-7-1-5)

国家药品标准制修订研究课题(2022Z16)

药品监管科学全国重点实验室课题(2023SKLDRS0102)

出版年

2024
中国现代中药
中国中药协会,中国医药集团总公司,中国药材公司

中国现代中药

CSTPCD
影响因子:0.65
ISSN:1673-4890
段落导航相关论文