首页|UPLC-MS/MS测定九味羌活颗粒中7个马兜铃酸类成分

UPLC-MS/MS测定九味羌活颗粒中7个马兜铃酸类成分

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目的:采用超高效液相色谱-质谱法(UPLC-MS/MS)同时测定九味羌活颗粒中 7 个马兜铃酸类成分的含量.方法:采用Shim-pack Velox PFPP 色谱柱(100 mm×2.1 mm,1.8 μm),以 1 mmol·L-1 甲酸铵溶液(含0.05%甲酸,A)-甲醇(B)为流动相梯度洗脱.体积流量为 0.4 mL·min-1,柱温为 40℃,进样量为 1 μL,电喷雾离子源,多反应监测模式.结果:7 个马兜铃酸类成分线性关系良好,r均≥0.997,加样回收率为 86.5%～112.2%;检出限为 0.05～0.31 ng·mL-1,定量限为 0.18～1.04 ng·mL-1.对 3 个企业 8 批样品进行测定,结果检出马兜铃酸Ⅳa、马兜铃内酰胺的质量分数分别为 0～0.417、0.021～0.173 μg·g-1.结论:该方法重复性好、灵敏度高,可用于九味羌活颗粒中马兜铃酸类成分的测定.
Simultaneous Determination of 7 Aristolochic Acids of Jiuwei Qianghuo Granules by UPLC-MS/MS
Objective:To establish an ultra high-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of seven aristolochic acid compounds in Jiuwei Qianghuo Granules.Method:The chromatographic separation was performed on a Shim-pack Velox PFPP column(100 mm×2.1 mm,1.8 μm),and gradient elution was carried out with 1 mmol·L-1 ammonium formate(containing 0.05%formic acid,solution A)and methanol(solution B)as the mobile phase.The column temperature was set at 40℃,and injection volume was 1 μL with volumetric flow rate of 0.4 mL·min-1.The scanning was performed using electrospray ionization(ESI)source in multiple reaction monitoring(MRM)mode and positive ion mode.Results:The linearity of aristolochic acid components was good.The correlation coefficient of standard curve was≥0.997,and the accuracy ranged from 86.5%to 112.2%.The limits of detection were between 0.05 and 0.31 ng·mL-1,and the limits of quantification were between 0.18 and 1.04 ng·mL-1.aristolochic acid Ⅳa and aristololactam were detected in 8 batches of samples from three enterprises,and the mass fractions were 0-0.417 μg·g-1 and 0.021-0.173 μg·g-1,respectively.Conclusion:The method has good repeatability and high sensitivity,and can be used for the determination of aristolochic acids in Jiuwei Qianghuo Granules.

UPLC-MS/MSJiuwei Qianghuo Granulesaristolochic acid Ⅰaristolochic acid Ⅱaristolochic acid Ⅲaaristolochic acid Ⅳaaristolochic acid Ⅶaaristolochic acid Ⅲaristololactam

李舒琪、孙慧珠、苏建、王常顺、石丹姝、刘永利

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河北中医药大学,河北 石家庄 050200

河北省药品医疗器械检验研究院 河北省中药质量评价与标准研究重点试验室,河北 石家庄 050227

岛津企业管理(中国)有限公司,北京 100020

超高效液相色谱-质谱法 九味羌活颗粒 马兜铃酸Ⅰ 马兜铃酸Ⅱ 马兜铃酸Ⅲa 马兜铃酸Ⅳa 马兜铃酸Ⅶa 马兜铃酸Ⅲ 马兜铃内酰胺

国家药品标准制修订研究课题河北省重点研发计划项目

2021Z16-421372502D

2024

10.13313/j.issn.1673-4890.20230728003

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
年,卷(期)：2024.26(8)