HPLC-ELSD法同时测定脑血栓片中胆酸、猪去氧胆酸和去氧胆酸的含量

Determination of Cholic Acid,Hyodeoxycholic Acid and Deoxycholate Acid in Naoxueshuan Tablet by HPLCELSD

目的：建立测定脑血栓片中胆酸、猪去氧胆酸和去氧胆酸含量的方法。方法：采用高效液相色谱-蒸发光散射检测法。色谱柱为SHIMADZU VP-ODS C18,检测器为蒸发光散射检测器,流动相为乙腈-0.2%甲酸水溶液（梯度洗脱）,流速为1.0 ml/min,柱温为30℃,进样量为10μl。结果：胆酸、猪去氧胆酸和去氧胆酸进样量分别在0.03984-0.3984、0.032064-0.32064、0.033952-0.33952 mg（r≥0.999 0）范围内进样量的对数值与其峰面积的对数值呈良好的线性关系;精密度、稳定性、重复性试验的RSD〈2%;加样回收率分别为101.33%-104.05%、95.56%-101.38%、96.07%-97.12%,RSD分别为0.95%、2.54%、0.44%（n=6）。结论：该方法简便、准确,适用于脑血栓片中胆酸、猪去氧胆酸和去氧胆酸的含量测定。

OBJECTIVE： To establish a method for the contents determination of cholic acid, hyodeoxycholic acid and deoxycholate acid in Naoxueshuan tablet. METHODS：HPLC-ELSD was performed on the column of SHIMADZU VP-ODS C18 with mobile phase of acetonitrile-0.2% formic acid（gradient elution）column temperature was 30 ℃, at flow rate of 1.0 ml/min, and the volume injection was 10μl. RESULTS：The linear range was 0.039 84-0.398 4 mg for cholic acid, 0.032 064-0.320 64 mg for hyode-oxycholic acid and 0.0339 52-0.339 52 μg for deoxycholate acid（r≥0.999 0）,and the logarithm value of volume injection and peak area showed good linear relationship; RSDs of precision, stability and reproducibility tests were lower than 2 % ; recoveries were 101.33%-104.05% （RSD=0.95%, n=6）, 95.56%-101.38% （RSD=2.54%, n=6） and 96.07%-97.12% （RSD=0.44%, n=6）, respectively. CONCLUSIONS ： The method is simple and accurate, and suitable for the contents determination of cholic acid, hyodeoxycholic acid and deoxycholate acid in Naoxueshuan tablet.