中国现代中药2024,Vol.26Issue(8) :1326-1331.DOI:10.13313/j.issn.1673-4890.20230615001

超高效液相色谱串联质谱法测定木香马兜铃中马兜铃酸Ⅰ及马兜铃酸Ⅱ的含量

Content Determination of Aristolochic Acid Ⅰ and Aristolochic Acid Ⅱ in Aristolochia moupinensis Franch.by UPLC-MS/MS

罗疆南 李靖云 王欢 王子昕 丁野 孙辉 李文莉 刘静 戴忠 马双成
中国现代中药2024,Vol.26Issue(8) :1326-1331.DOI:10.13313/j.issn.1673-4890.20230615001

超高效液相色谱串联质谱法测定木香马兜铃中马兜铃酸Ⅰ及马兜铃酸Ⅱ的含量

Content Determination of Aristolochic Acid Ⅰ and Aristolochic Acid Ⅱ in Aristolochia moupinensis Franch.by UPLC-MS/MS

罗疆南 1李靖云 1王欢 1王子昕 1丁野 1孙辉 1李文莉 1刘静 2戴忠 2马双成2
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作者信息

  • 1. 湖南省药品检验检测研究院,湖南 长沙 410001;湖南省药品质量评价工程技术研究中心,湖南 长沙 410001
  • 2. 中国食品药品检定研究院,北京 100050
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摘要

目的:建立测定木香马兜铃中马兜铃酸Ⅰ(AA-Ⅰ)及AA-Ⅱ含量的超高效液相色谱-质谱法.方法:色谱柱为Agilent Poroshell SB-C18(100 mm×2.1 mm,2.7 μm),流动相为乙腈-0.1%甲酸水溶液(含 5 mmol·L-1 甲酸铵),梯度洗脱,流速 0.3 mL·min-1,柱温 35℃,离子源为电喷雾离子源,扫描方式为正离子扫描,多反应离子监测模式.结果:AA-Ⅰ在质量浓度为 1.036~207.310 ng·mL-1时与峰面积线性关系良好(r=0.999 5);AA-Ⅱ在质量浓度为1.1~110.0 ng·mL-1时与峰面积线性关系良好(r=0.999 1);AA-Ⅰ的定量限、检测限分别为0.328 7、0.098 6 pg;AA-Ⅱ的定量限、检测限分别为 0.650 6、0.195 2 pg;AA-Ⅰ的精密度、稳定性、重复性试验RSD均小于 5.0%;AA-Ⅱ的精密度、稳定性、重复性试验RSD均小于 5.0%;AA-Ⅰ的平均加样回收率为 92.50%,RSD为 4.3%;AA-Ⅱ的平均加样回收率为 104.97%,RSD为 3.7%.15批木香马兜铃药材中 1批未检出AA-Ⅰ,8批未检出AA-Ⅱ,其余批次的AA-Ⅰ质量分数为 5.94×10-4~2.86 mg·g-1,AA-Ⅱ质量分数为 0.09~0.50 mg·g-1.结论:所建立的方法专属性强、快速、灵敏,可用于木香马兜铃中AA-Ⅰ及AA-Ⅱ的含量测定.

Abstract

Objective:To establish an ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the content determination of aristolochic acid Ⅰ(AA-Ⅰ)and AA-Ⅱ in Aristolochia moupinensis Franch.Methods:The chromatographic column was Agilent Poroshell SB-C18 column(100 mm×2.1 mm,2.7 μm);the mobile phase was acetonitrile-0.1%formic acid aqueous solution(containing 5 mmol·L-1 ammonium formate)with gradient elution;the flow rate was 0.3 mL·min-1;the column temperature was 35℃;the ion source was electrospray ion source;the scanning mode was positive ion scanning with multiple reaction monitoring(MRM)mode.Results:AA-Ⅰshowed a good linear relationship with the peak area at a mass concentration of 1.036-207.310 ng·ml-1(r=0.999 5).AA-Ⅱshowed a good linear relationship with the peak area at a mass concentration of 1.1-110.0 ng·ml-1(r=0.999 1).The limit of quantification(LOQ)and limit of detection(LOD)of AA-Ⅰ were 0.328 7 and 0.098 6 pg,respectively,and the LOQ and LOD of AA-Ⅱ were 0.650 6 and 0.195 2 pg,respectively.The RSDs of precision,stability and repeatability tests of AA-Ⅰwere all less than 5.0%,and those of AA-Ⅱ were all less than 5.0%.The average spiked recovery of AA-Ⅰ was 92.50%with RSD of 4.3%.The average spiked recovery of AA-Ⅱ was 104.97%with RSD of 3.7%.Among the 15 batches of A.moupinensis Franch,no AA-Ⅰ was detected in 1 batch,and no AA-Ⅱ was detected in 8 batches.The content of AA-Ⅰ in the remaining batches was 5.94×10-4-2.86 mg·g-1,and that of AA-Ⅱ was 0.09-0.50 mg·g-1.Conclusion:The established method is specific,rapid,sensitive,and can be used for the content determination of AA-Ⅰ and AA-Ⅱ in A.moupinensis Franch..

关键词

马兜铃酸Ⅰ/马兜铃酸Ⅱ/超高效液相色谱-质谱法/木香马兜铃/含量测定

Key words

aristolochic acid Ⅰ/aristolochic acid Ⅱ/UPLC-MS/MS/Aristolochia moupinensis Franch./content determination

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基金项目

2022年度国家药品标准制修订研究课题(2021Z15-2)

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
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