UPLC-MS/MS测定九味羌活颗粒中7个马兜铃酸类成分  

Simultaneous Determination of 7 Aristolochic Acids of Jiuwei Qianghuo Granules by UPLC-MS/MS

作　　者：李舒琪 孙慧珠 苏建 王常顺 石丹姝 刘永利 LI Shu-qi;SUN Hui-zhu;SU Jian;WANG Chang-shun;SHI Dan-Shu;LIU Yong-li(Hebei University of Chinese Medicine,Shijiazhuang 050200,China;Hebei Key Laboratory of Traditional Chinese Medicine Quality Evaluation and Standard Research,Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050227,China;Shimadzu(China)Co.,Ltd.,Beijing,100020,China)

机构地区：[1]河北中医药大学,河北石家庄050200 [2]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 [3]岛津企业管理(中国)有限公司,北京100020

出　　处：《中国现代中药》2024年第8期1300-1306,共7页Modern Chinese Medicine

基　　金：国家药品标准制修订研究课题(2021Z16-4);河北省重点研发计划项目(21372502D)。

摘　　要：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,1.8μm),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1μL,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、0.021~0.173μg·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。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,1.8μm),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 1μL 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 acidⅣa and aristololactam were detected in 8 batches of samples from three enterprises,and the mass fractions were 0-0.417μg·g^(–1) and 0.021-0.173μg·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.

关 键 词：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 

分 类 号：R282[医药卫生—中药学]