首页|UPLC-MS/MS测定3种川芎茶调类制剂中马兜铃酸Ⅰ的含量

UPLC-MS/MS测定3种川芎茶调类制剂中马兜铃酸Ⅰ的含量

扫码查看
目的:建立超高效液相色谱-质谱法(UPLC-MS/MS)同时测定川芎茶调丸、川芎茶调丸(浓缩丸)、川芎茶调颗粒中马兜铃酸Ⅰ的含量,对不同剂型中马兜铃酸Ⅰ的含量进行比较.方法:采用ACQUITY UPLC BEH C18 色谱柱(100 mm×2.1 mm,1.7 μm);以乙腈-0.1%甲酸水溶液为流动相梯度洗脱,流速为 0.3 mL·min-1,电喷雾离子源,多反应监测,选择m/z 359.0→298.1 和 359.0→296.1 离子对进行监测,对精密度、稳定性、重复性等进行验证的同时,对 3种剂型共 48批样品进行测定.结果:马兜铃酸Ⅰ在质量浓度为 2.96~295.82 ng·mL-1时与峰面积线性关系良好,r均大于 0.999,平均回收率分别为 93.36%、85.08%、90.13%,RSD分别为 10.04%、6.04%、11.85%,定量限为 0.040 6~0.157 7 μg·g-1.结论:该方法准确度、精密度、稳定性、线性关系良好,适用于川芎茶调类制剂中马兜铃酸Ⅰ的检测和分析;对于含有马兜铃酸类毒性成分中药的中药制剂更宜采用非原粉入药的方式.
Content Determination of Aristolochic Acid Ⅰ in Three Chuanxiong Chatiao Products by UPLC-MS/MS
Objective:An analytical method was established to simultaneously determine and compare the content of aristolochic acid Ⅰ in three dosage forms of Chuanxiong Chatiao products,Chuanxiong Chatiao Pills,Chuanxiong Chatiao Pills(concentrated pills)and Chuanxiong Chatiao Granules,by ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).Methods:The samples were separated on ACQUITY UPLC BEH C18(100 mm×2.1 mm,1.7 μm)column and gradient elution was performed with acetonitrile-0.1%formic acid solution as a mobile phase.The flow rate was 0.3 mL·min-1,and triple quadrupole tandem mass spectroscopy was used as the detector.The samples were detected under multiple reaction monitoring(MRM)mode with electrospray ionization(ESI)in positive ion mode,and the mass to charge ratio(m/z)359.0→298.1 and 359.0→296.1 ion pairs were selected for monitoring.The contents of aristolochic acid Ⅰin three Chuanxiong Chatiao products from 48 batches were determined and the precision,stability and repeatability were verified.Results:The contents of aristolochic acid Ⅰ had a good linear relationship with the peak area when the mass concentration was 2.96-295.82 ng·mL-1,and the r value of the three products were all greater than 0.999.The average recoveries were 93.36%,85.08%,90.13%,and RSDs were10.04%,6.04%,11.85%,respectively.The limit of quantitation(LOQ)was 0.040 6-0.157 7 μg·g-1.Conclusion:This method has good accuracy,precision,stability and linearity,and is suitable for the detection and analysis of aristolochic acid Ⅰ in Chuanxiong Chatiao preparation.The results suggest that for the processing and preparation of traditional Chinese medicine containing toxic components such as aristolochic acid,it is more appropriate to use non original powder as the medicine.

Chuanxiong Chatiao serial productsdosage formUPLC-MS/MSaristolochic acid Ⅰcontent determination

李青、苏晶、丁慧宁

展开 >

重庆市药品技术审评查验中心,重庆 401120

重庆市食品药品检验检测研究院 重庆市药物过程与质量控制工程技术研究中心,重庆 401121

上海中医药大学 中药学院,上海 201203

川芎茶调类制剂 剂型 超高效液相色谱-质谱法 马兜铃酸Ⅰ 含量测定

国家药典委员会"含细辛中成药标准修订"项目

2021Z16

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
年,卷(期):2024.26(8)