双参通脉滴丸制备中7种有效成分快速质量监测的HPLC-MS法  

A rapid quality control method for seven marker components in Shuangsen Tongmai Dripping Pill by HPLC-MS

作　　者：陈晓莉[1] 王骊丽[2] 王文鹏[2] 吴寅[1] 王婧雯[1] 杨春娥[1] 

机构地区：[1]第四军医大学西京医院药剂科,陕西西安710032 [2]西北大学合成与天然功能分子化学教育部重点实验室,西北大学现代分离科学研究所,陕西西安710069

出　　处：《中成药》2010年第6期953-957,共5页Chinese Traditional Patent Medicine

基　　金：陕西省科学技术研究发展计划社发攻关项目(No.2006k10-2G(2))

摘　　要：目的:进行双参通脉滴丸(人参、丹参、川芎)制备的质量快速监测。方法:采用高效反相液相色谱(RP-HPLC)和MALDI-TOF-MS法,以丹参酮ⅡA含量作为指标,色谱柱为C18-ODS(150mm×4.6mmI.D.,5μm,岛津公司),以乙腈(含0.5%冰醋酸)和水(含0.5%冰醋酸)体系为流动相,流速为1mL/min时,柱温为25℃。结果:波长为203nm,可同时测定到人参皂苷Rg1、人参皂苷Rb1、人参皂苷Re和丹参酮ⅡA。波长为270nm,可同时测定到制剂中的川芎嗪,丹酚酸B,阿魏酸,丹参酮ⅡA4种单体的有效成分,并在其测定的范围内均具有良好的线性关系。用MALDI-TOF-MS分析鉴定样品中丹参酮IIA的分子量一致。结论:该方法快速、准确、其精密度、稳定性和重现性良好,对双参通脉滴丸中7种化学成分均能成功地达到质量监测。AIM： To improve the safety,efficacy,stability,and controllability of Shuangshen Tongmai Dripping Pill（Radix et Rhizoma Ginseng,Radix et Rhizoma Salviae miltiorrhizae,Rhizoma Chuanxiong）.METHODS： In this study,RP-HPLC and MALDI-TOF-MS were used to establish a method for rapid quality control of Shuangsen Tongmai Dripping Pill,with the amount of tanshinone ⅡA as a marker.C18-ODS column（150 mm × 4.6 mm I.D.5 μm,shimadzu） was adopted with the mobile phase of a mixture of acetonitrile and 0.5 acetic acid in gradient elution mode,at a flow rate of 1.0 mL/min and column temperature at 25 ℃.RESULTS： With the detection wavelength at 203 nm,ginsenoside Rg1,Rb1 and Re,tanshinone ⅡA could be simultaneously assayed.With the detection wavelength at 270 nm,tanshone ⅡA,salvianolic acid B,ferulic acid,and chuanxiongzine could be simultaneously assayed.Regression equations revealed good linear relationship between the peak areas of the constituents and their concentration ranges.MALDI-TOF-MS analysis showed the identical molecular weight of tanshinone ⅡA among samples.CONCLUSION： The method is rapid and accurate with good resolution,stability and reproducibility and could be used to monitor seven marker components in Shuangsen Tongmai Dripping Pill quantitatively.The proposed method could also be used for the quality monitoring of other products containing Radix et Rhizoma Ginsong and Radix et Rhizoma Salviae Miltiorrhizae,or Radix et Rhizoma Salviae Miltiorrhizae and Rhizoma Chuanxiong,and for the in vivo pharmacodynamical and pharmacokenetical studies.

关 键 词：双参通脉滴丸 制备 反相高效液相色谱-MALDI-TOF-MS法 质量监测 

分 类 号：R927.2[医药卫生—药学]