HPLC-MS法测定首乌丸中五种蒽醌类成分的含量

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。

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

Purpose To establish a HPLC-MS method for the determination of five phenolic compounds in Shouwu Pills.Methods The five phenolic compounds—rhein,aloe-emodin,emodin,chrysophanol and physcion were separated on Phenomenex Luna 3 μm C18(150 mm×2 mm) column and detected 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 separation of phenolic compounds-rhein,aloe-emodin,emodin,chrysophanol and physcion.The average recoveries 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=1.27%),and 105.4%(RSD=1.54%) respectively,in addition to that the five total ones separately were 99.67%(RSD=1.12%),99.21%(RSD=1.78%),98.94%(RSD=1.23%),98.32%(RSD=2.08%),and 96.10%(RSD=2.67%) respectively.Conclusion This method is accurate,simple and rapid.This study provides the reference to establish the quality standard for Shouwu Pills.