HPLC-MS法同时测定消炎利胆片中6种化学成分含量研究

Simultaneous quantitive determination of six chemical compositions in Xiaoyan Lidan Pian by HPLC-MS

目的建立一种快速同时测定消炎利胆片中6种主要有效成分穿心莲内酯、脱水穿心莲内酯、拉西多宁、表诺多醇、冬凌草甲素和表诺多星含量的液相色谱-质谱联用(HPLC-MS)法。方法采用HPLC-MS,Dikma Diamonsil C18(250 mm×4.6 mm,5μm)色谱柱;甲醇-0.5‰甲酸水梯度洗脱。采用电喷雾离子源(ESI);正离子模式监测;多反应离子监测模式定量,6种被测成分的监测离子对分别为351.3/257.3(穿心莲内酯)、333.2/257.3(脱水穿心莲内酯)、365.3/347.3(拉西多宁、表诺多醇、冬凌草甲素)和363.3/281.3(表诺多星)。结果消炎利胆片中待测6个化学成分在15min内完全分离,方法的线性关系、线性范围、精密度及稳定性较好,回收率(n=3)分别为101.3%,98.5%,99.4%,100.3%,100.4%和99.4%。结论该方法简便、快速、准确、专属性高,可用于消炎利胆片的质量控制。

Objective To establish a quick method for simultaneous quantitative determination of six chemical compositions in Xiaoyan Lidan Plan, including andrographolide, dehydroandrographolide, lasiodonin, epinodosinol, oridonin and epinodosin, by HPLC-MS. Methods The procedure of HPLC- MS was performed on the chromatographic column of Dikma Diamonsil C18 （250 mm × 4.6 mm, 5 μm） , and the mobile phase was methanol-0.5%v formic acid solution. Electrospray ionization （ESI） source, monitoring in positive ion mode and multiple reaction monitoring （MRM） were applied for the quantitative determination. The monitoring ion pairs of 6 detected compositions were, respectively, 351. 3/257.3 （ andrographolide ）, 333.2/257.3 （ dehydroandrographolide ）, 365. 3/347. 3 （ lasiodonin, epinodosinol and oridonin） and 363.3/281.3 （epinodosin）. Results Six chemical compositions in Xiaoyan Lidan Pian were separated totally within 15 minutes, and the linear relationships, linear ranges, precision and stability of the method were good. The average recovery （n = 3 ） was, respectively, 101. 3%, 98.5%, 99.4%, 100.3% accurate with higher specificity, , 100.4% and 99.4%. Conclusion The method is simple, rapid, which can be used for the quality control of Xiaoyan Lidan Pian.