摘要:
OBJECTIVE:To establish a method for the simultaneous determination of rhein,emodin,chrysophanol and phy-scion in Niuhuang shangqing pill. METHODS:HPLC was performed on the column was Kromasil C18 with mobile phase of metha-nol-0.5% phosphoric acid(75:25,V/V),the column temperature was 30 °C,the flow rate was 1.0 ml/min,the detection wave-length was 230 nm,and the injection volume was 10μl. RESULTS:The linear range was 1.50-150 mg/L for rhein,0.95-95 for em-odin,1.30-130 for chrysophanol and 1.15-115 mg/L for physcion(r≥0.995 0);RSDs of precision,stability and reproducibility tests were lower than 2%;recoveries were 97.03%-100.40%(RSD=1.23%,n=9),98.37%-102.50%(RSD=1.15%,n=9),98.03%-101.10%(RSD=1.05%,n=9)and 97.83%-104.50%(RSD=2.16%,n=9). CONCLUSIONS:The method is simple,stable with good re-producibility,and can be used for the contents determination of rhein,emodin,chrysophanol and physcion in Niuhuang shangqing pill.%目的:建立同时测定牛黄上清丸中大黄酸、大黄素、大黄酚、大黄素甲醚4种蒽醌类化合物含量的方法.方法:采用高效液相色谱法.色谱柱为Kromasil C18,流动相为甲醇-0.5%磷酸(75:25,V/V),流速为1.0 ml/min,检测波长为230 nm,柱温为30°C,进样量为10μl.结果:大黄酸、大黄素、大黄酚、大黄素甲醚检测质量浓度线性范围分别为1.50~150、0.95~95、1.30~130、1.15~115 mg/L(r≥0.995 0);精密度、稳定性、重复性试验的RSD<2%;加样回收率分别为97.03%~100.40%(RSD=1.23%,n=9)、98.37%~102.50%(RSD=1.15%,n=9)、98.03%~101.10%(RSD=1.05%,n=9)、97.83%~104.5%(RSD=2.16%,n=9).结论:该方法操作简便、稳定、重复性好,可用于牛黄上清丸中大黄酸、大黄素、大黄酚、大黄素甲醚4种蒽醌类化合物含量的测定.