HPLC法同时测定牛黄上清丸中4种蒽醌类化合物的含量

Simultaneous Determination of Four Anthraquinone Compounds in Niuhuang Shangqing Pill by HPLC

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℃,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。

OBJECTIVE： To establish a method for the simultaneous determination of rhein, emodin, chrysophanol and physcion in Niuhuang shangqing pill. METHODS：HPLC was performed on the column was Kromasil CL8 with mobile phase of metha- nol-0.5% phosphoric acid（75 ： 25, V/V）, the column temperature was 30 %, the flow rate was 1.0 ml/min, the detection wavelength was 230 nm, and the injection volume was 10 μl. RESULTS： The linear range was 1.50-150 mg/L for rhein, 0.95-95 for emodin, 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 reproducibility, and can be used for the contents determination of rhein, emodin, chrysophanol and physcion in Niuhuang shangqing pill.