UPLC-MS/MS法同时测定通塞脉微丸中10种有效成分  

Simultaneous determination of ten effective components in Tongsaimai Pellets by UPLC-MS/MS

作　　者：程健[1] 狄留庆[1,2] 李俊松[1,2] 赵晓莉[1,2] 周伟[1] 

机构地区：[1]南京中医药大学药学院,江苏南京210046 [2]江苏省中药高效给药系统工程技术研究中心,江苏南京210046

出　　处：《中草药》2014年第5期659-664,共6页Chinese Traditional and Herbal Drugs

基　　金：国家自然科学基金资助项目(81073071);江苏省"青蓝工程"科技创新团队支持计划[(2008)30号];江苏省优势学科支持计划(ysxk-2010)

摘　　要：目的建立同时测定通塞脉微丸中10种有效成分（绿原酸、芹糖甘草苷、毛蕊异黄酮苷、木犀草苷、甘草苷、阿魏酸、异甘草苷、哈巴俄苷、甘草素和肉桂酸）的超高效液相色谱．串联质谱（UPLC-MS／MS）分析方法。方法采用BEHC18（100mmX2．1mm，1．7gm）色谱柱，流动相为乙腈．0．1％甲酸水溶液，梯度洗脱，体积流量为0_3mL／min，采用电喷雾电离源（ESI），多反应离子监测（MRM）扫描方式进行检测。结果10种成分线性关系分别为绿原酸Y=294．09肿17624；芹糖甘草苷Y=19．296x＋748．42；毛蕊异黄酮苷Y=670．8x＋11121；木犀草苷Y=490．45Ⅸ＋2938．3；甘草苷y=33．489x＋555；阿魏酸y=127．76x＋1343．5；异甘草苷y=57．87X＋804．81；哈巴俄苷y=13．125X-20．365：甘草素Y=29．057x＋367．71；肉桂酸y=72．867x＋1301．5，且各相关系数（r）均大于0．9990。精密度、重复性和稳定性良好；加样回收率在96．00％104．67％，RSD值均小于3％。结论所建立的方法准确、快捷，重复性好，可用于通塞脉微丸中绿原酸、芹糖甘草苷、毛蕊异黄酮苷、木犀草苷、甘草苷、阿魏酸、异甘草苷、哈巴俄苷、甘草素和肉桂酸10种有效成分的同时测定。Objective To establish a UPLC-MS/MS method for simultaneously determining ten components （chromogenic acid, liquiritin apioside, calycosin-7-glucoside, cynaroside, liquiritin, ferulic acid, isoliquiritoside, harpagoside, liquiritigenin, and cinnamic acid） in Tongsaimai Pellets. Methods A method for the simultaneous determination of the ten components was established by UPLC-MS/MS. The analysis was performed on a Waters Acquity BEH C18 column （100 mm × 2.1 mm, 1.7 μm） with the mixture of acetonitrile and 0.1% formic acid/water as mobile phase, and the gradient elution at a flow rate of 0.3 mL/min. The analytes were detected by tandem mass spectrometry with the electrospray ionization （ESI） source combined with multiple reaction monitoring （MRM） mode. Results The linear relationships between the concentration and peak areas of the ten components were chromogenic acid Y = 294.09 X ＋ 17 624; liquiritin apioside Y = 19.296 X ＋ 748.42; calycosin-7-glucoside Y = 670.8 X ＋ 11 121; cynaroside Y = 490.45 X ＋ 2 938.3; liquiritin Y = 33.489 X ＋ 555; ferulic acid Y = 127.76 X ＋ 1 343.5; isoliquiritoside Y = 57.87X ＋ 804.81; harpagoside Y = 13.125 X--20.365; liquiritigenin Y = 29.057 X ＋ 367.71; cinnamic acid Y = 72.867 X ＋ 1 301.5 （r 〉 0.999 0）; The precisions, repeatabilities, and stabilities of the method were satisfactory, and the average recoveries were between 96.00% and 104.67% with the relative standard deviations no more than 3%. Conclusion The established method is specific, rapid, and accurate for the determination of the ten effective components in Tongsaimai Pellets.

关 键 词：超高效液相色谱-串联质谱 通塞脉微丸 绿原酸 芹糖甘草苷 毛蕊异黄酮苷 木犀草苷 甘草苷 阿魏酸 异 甘草苷 哈巴俄苷 甘草素 肉桂酸 

分 类 号：R286.02[医药卫生—中药学]