液质联用法测定十一味参芪片中马兜铃酸Ⅰ、马兜铃酸Ⅳa和马兜铃内酰胺Ⅰ
投稿时间:2023-02-07     点此下载全文
引用本文:覃丽郦,何颂华,白桂昌,罗轶.液质联用法测定十一味参芪片中马兜铃酸Ⅰ、马兜铃酸Ⅳa和马兜铃内酰胺Ⅰ[J].中国现代中药,2023,25(12):2606-2611
DOI:10.13313/j.issn.1673-4890.20230207001
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作者中文名作者英文名单位中文名单位英文名E-Mail
覃丽郦 QIN Li-li 广西壮族自治区食品药品检验所 国家药品监督管理局中药材质量监测与评价重点实验室, 广西 南宁 530021 NMPA Key Laboratory for Quality Monitoring and Evaluation of Traditional Chinese Medicine,Chinese Material Medica, Guangxi Institute for Food and Drug Control, Nanning 530021, China  
何颂华 HE Song-hua 广西壮族自治区食品药品检验所 国家药品监督管理局中药材质量监测与评价重点实验室, 广西 南宁 530021 NMPA Key Laboratory for Quality Monitoring and Evaluation of Traditional Chinese Medicine,Chinese Material Medica, Guangxi Institute for Food and Drug Control, Nanning 530021, China  
白桂昌* BAI Gui-chang 广西壮族自治区食品药品检验所 国家药品监督管理局中药材质量监测与评价重点实验室, 广西 南宁 530021 NMPA Key Laboratory for Quality Monitoring and Evaluation of Traditional Chinese Medicine,Chinese Material Medica, Guangxi Institute for Food and Drug Control, Nanning 530021, China  
罗轶* LUO Yi 广西壮族自治区食品药品检验所 国家药品监督管理局中药材质量监测与评价重点实验室, 广西 南宁 530021 NMPA Key Laboratory for Quality Monitoring and Evaluation of Traditional Chinese Medicine,Chinese Material Medica, Guangxi Institute for Food and Drug Control, Nanning 530021, China  
中文摘要:目的 建立十一味参芪片中马兜铃酸Ⅰ、马兜铃酸Ⅳa和马兜铃内酰胺Ⅰ的液相色谱-质谱法(LC-MS)检测分析方法。方法 Kromasil Proshell C18色谱柱(100 mm×2.1 mm,2.5 μm),以乙腈-0.1%乙酸水溶液(含10 mmol·L–1乙酸铵)为流动相,梯度洗脱,流速0.3 mL·min–1;多反应监测模式,马兜铃酸Ⅰ为m/z 359.1→298.1(定量)和m/z 359.1→296.1(定性),马兜铃酸Ⅳa为m/z 375.1→312.2(定量)和m/z 375.1→297.2(定性),马兜铃内酰胺Ⅰ为m/z 294.1→279.0(定量)和m/z 294.1→251.1(定性),建立十一味参芪片中3个马兜铃酸类成分的LC-MS,在方法学验证的基础上对所有样品进行检测分析。结果 马兜铃酸Ⅰ、马兜铃酸Ⅳa和马兜铃内酰胺Ⅰ进样量分别在2.019 7~100.982 9、1.947 8~116.865 6、1.971 8~98.588 0 pg时线性关系良好(r>0.999),定量限分别为1、6、2 pg,加样回收率分别为92.95%(RSD为2.28%)、80.09%(RSD为4.16%)、104.89%(RSD为3.24%)。14批十一味参芪片样品中马兜铃酸Ⅰ、马兜铃酸Ⅳa和马兜铃内酰胺Ⅰ的检出量分别为21.0~47.6、185.0~506.1、164.4~426.0 ng·g–1结论 所建立的方法快速、准确、灵敏、可靠,能够用于十一味参芪片中上述马兜铃酸类成分的筛查与分析,可为其安全性有关成分研究提供参考。
中文关键词:十一味参芪片  马兜铃酸Ⅰ  马兜铃酸Ⅳa  马兜铃内酰胺Ⅰ  液相色谱-质谱法
 
Determination of Aristolochic Acid , Aristolochic Acid Ⅳa, and Aristolactam in Shiyiwei Shenqi Tablets by Liquid Chromatography-mass Spectrometry
Abstract:Objective To establish a liquid chromatography-mass spectrometry (LC-MS) method for the detection and analysis of aristolochic acid Ⅰ, aristolochic acid Ⅳa, and aristolactam Ⅰ in Shiyiwei Shenqi Tablets.Methods A Kromasil Proshell C18 chromatographic column (100 mm×2.1 mm, 2.5 μm) was used with acetonitrile-0.1% acetic acid solution (containing 10 mmol·L–1 ammonium acetate) as the mobile phase, using a gradient elution at a flow rate of 0.3 mL·min–1. Multiple reaction monitoring mode was employed with m/z 359.1→298.1 (quantitative) and m/z 359.1→296.1 (qualitative) for aristolochic acid Ⅰ, m/z 375.1→312.2 (quantitative) and m/z 375.1→297.2 (qualitative) for aristolochic acid Ⅳa, and m/z 294.1→279.0 (quantitative) and m/z 294.1→251.1 (qualitative) for aristolactam Ⅰ. The LC-MS method for the three components in Shiyiwei Shenqi Tablets was established, and all samples were subsequently subjected to detection and analysis based on methodological verification.Results The linear relations of aristolochic acid Ⅰ, aristolochic acid Ⅳa, and aristolactam Ⅰ were good with injection volumes of 2.019 7-100.982 9, 1.947 8-116.865 6, and 1.971 8-98.588 0 pg, respectively, with correlation coefficients (r) greater than 0.999. The respective limits of quantification were 1, 6, 2 pg. The recoveries of the three components were 92.95% (RSD 2.28%), 80.09% (RSD 4.16%), and 104.89% (RSD 3.24%), respectively. The detected levels of aristolochic acid Ⅰ, aristolochic acid Ⅳa, and aristolactam Ⅰ in the 14 batches of Shiyiwei Shenqi Tablets were 21.0-47.6, 185.0-506.1, and 164.4-426.0 ng·g–1, respectively.Conclusion The established LC-MS method is rapid, accurate, sensitive, and reliable, and can be used for the screening and analysis of the above components in Shiyiwei Shenqi Tablets, providing reference data for research on their safety-related components.
keywords:Shiyiwei Shenqi Tablets  aristolochic acidⅠ  aristolochic acid Ⅳa  aristolactamⅠ  LC-MS
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