超高效液相-质谱法测定滴通鼻炎水中马兜铃酸Ⅰ、Ⅱ的含量
Content determination of aristolochic acid Ⅰ and aristolochic acid Ⅱ in Ditong Biyan Shui by UPLC-MS/MS
郭日新 1肖萌 1刘静 1戴忠 1马双成1
作者信息
- 1. 中国食品药品检定研究院中药民族药检定所,北京 100050
- 折叠
摘要
目的 测定滴通鼻炎水中马兜铃酸Ⅰ、马兜铃酸Ⅱ的含量,为其质量控制提供借鉴.方法 采用超高效液相-质谱法(UPLC-MS/MS)同时测定滴通鼻炎水中马兜铃酸Ⅰ、马兜铃酸Ⅱ的含量.色谱柱采用Waters-ACQUI UPLC HSS T3 C18(2.1 mm×100 mm,1.8μm),采用乙腈为流动相A,0.1%甲酸含1 mmol·L-1 乙酸铵溶液为流动相B,梯度洗脱,电喷雾离子源(ESI),正离子多反应监测模式,以标准曲线法计算含量.结果 17批滴通鼻炎水中有9批样品未检出马兜铃酸Ⅰ(检出限 0.13 pg),8 批样品中检出马兜铃酸Ⅰ,含量在0.41～3.60 ng·mL-1.所有样品中均未检出马兜铃酸Ⅱ(检出限 0.41 pg).结论 建立了UPLC-MS/MS同时测定滴通鼻炎水中马兜铃酸Ⅰ、马兜铃酸Ⅱ含量的方法,该方法专属性强、灵敏度高、重复性好,可为滴通鼻炎水中马兜铃酸Ⅰ、马兜铃酸Ⅱ的质量控制提供参考.
Abstract
Objective To determine the contents of aristolochic acid Ⅰ and aristolochic acid Ⅱ in Ditong Biyan Shui,and to provide reference for quality control.Methods A UPLC-MS/MS method was established to determine the contents of aristolochic acid Ⅰ and aristolochic acid Ⅱ.An Waters-ACQUI UPLC HSS T3 C18(2.1 mm×100 mm,1.8 μm)was used as the chromatographic column.The mobile phase was eluted with acetonitrile(A),0.1%formic acid solution(B)using a gradient elution method.The electrospray spray ion source(ESI)and positive ion multi-reaction monitoring mode were adopted.The contents were calculated using the standard curve method.Results Aristolochic acid Ⅰ was not detected in 9 samples of 17 batches of Ditong Biyan Shui(detection limit 0.13 pg),but was detected in 8 batches of samples,with the contents ranging from 0.41 to 3.60 ng·mL-1.Aristolochic acid Ⅱ was not detected in any of the samples(detection limit 0.41 pg).Conclusion A UPLC-MS/MS method has been established to determine the contents of aristolochic acid Ⅰ and aristolochic acid Ⅱ in Ditong Biyan Shui,with high specificity,high sensitivity,good repeatability,which can provide reference for quality control of aristolochic acid Ⅰ and aristolochic acid Ⅱ in Ditong Biyan Shui.
关键词
滴通鼻炎水/马兜铃酸Ⅰ/马兜铃酸Ⅱ/超高效液相-质谱法/含量测定Key words
Ditong Biyan Shui/aristolochic acid Ⅰ/aristolochic acid Ⅱ/UPLC-MS/MS/content determination引用本文复制引用
基金项目
"重大新药创制"科技重大专项(2018ZX09735-006)
国家药品标准制修订研究课题(2022)(2022Z16)
国家药品监督管理局药品监管科学体系建设重点项目(RS2024Z006)
出版年
2024
NETL
NSTL
万方数据