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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 Ⅰ, Aristolochic Acid Ⅳa, and Aristolactam Ⅰ 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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