HPLC-MS法测定首乌丸中五种蒽醌类成分的含量

Determination of the content of five phenolic compounds in Shouwu Pills by HPLC-MS-MS

目的建立首乌丸中芦荟大黄素、大黄酸、大黄素、大黄酚以及大黄素甲醚等五种蒽醌类成分的含量测定方法。方法 HPLC-MS联用法对首乌丸中五种蒽醌类物质的含量同时测定。色谱条件为:Phenomenex Luna C18(3μm,150 mm×2 mm)柱,流动相:甲醇-5 mmol/L醋酸铵溶液(90∶10),流速:0.2 mL/min,电喷雾型质谱检测器。结果大黄酸、芦荟大黄素、大黄素、大黄酚、大黄素甲醚分别在0.18～56.6,0.016～10.03,0.024～14.94,0.18～11.33,0.011～6.85 ng范围内线性良好;r分别为0.999 8,0.999 9,0.998 8,0.999 9,0.999 9;水解前平均回收率分别为108.5%(RSD=0.93%),98.67%(RSD=1.57%),100.2%(RSD=0.69%),99.73%(RSD=1.27%),105.4%(RSD=1.54%);水解后平均回收率分别为99.67%(RSD=1.12%),99.21%(RSD=1.78%),98.94%(RSD=1.23%),98.32%(RSD=2.08%),96.10%(RSD=2.67%)。结论此法简便、准确、快捷,可用于首乌丸的质量控制。

Purpose To establish a HPLC-MS method for the determination of five phenolic com- pounds in Shouwu Pills. Methods The five phenolic eompounds--rhein, aloe-emodin, emodin, chry- sophanol and physcion were separated on Phenomenex Luna 3 Ixm C18 （150 mm x 2 mm） column and de- tected by a spray electric detector, with methanol-5 mmol/L ammonium acetate （90： 10） as a mobile phase. Results There was good linearity from 0.18-56.6 ng（ r = 0. 999 8） ,0. 016-10.03 ng（ r = 0. 999 9）, 0. 024-14.94 ng（r =0. 998 8） ,0.18-11.33 ng（r =0. 999 9） ,0. 011-6.85 ng（r =0. 999 9） in separa- tion of phenolic compounds-rhein,aloe-emodin,emodin, chrysophanol and physcion. The average recover- ies of the five free phenolic compounds separately were 108.5% （RSD = 0.93% ） , 98.67% （RSD = 1.57%）,100.2%（RSD=0.69%）,99.73%（RSD=l.27%）,and 105.4%（RSD=l.54%） respec- tively,in addition to that the five total ones separately were 99.67% （RSD = 1.12% ） ,99.21% （RSD = 1.78%）,98.94%（RSD=l.23%）,98.32%（RSD=2.08%）,and 96.10%（RSD=2.67%） respec- tively. Conclusion This method is accurate, simple and rapid. This study provides the reference to estab- lish the quality standard for Shouwu Pills.