HPLC-ELSD法测定清开灵栓中胆酸和猪去氧胆酸的含量

目的:建立以高效液相色谱-蒸发光散射(HPLC-ELSD)检测法测定清开灵栓中胆酸和猪去氧胆酸含量的方法。方法:色谱柱为Diamonsil C18(250mm×4.6mm,5μm),流动相为0.1%甲酸-乙腈(梯度洗脱),ELSD检测器漂移管温度为110℃,氮气流速为2.0L·min-1。结果:胆酸和猪去氧胆酸的进样量分别在0.59～7.40μg(r=0.9996)、0.38～4.8μg(r=0.9997)范围内与各自峰面积积分值呈良好线性关系;二者平均回收率分别为99.20%和98.57%,RSD分别为1.4%(n=6)、1.8%(n=6)。结论:本方法简便、准确、分离效果好,可用于清开灵栓的质量控制。

Determination of Cholalic Acid and Hyodeoxycholic Acid in Qingkailing Suppository by HPLC- ELSD

OBJECTIVE： To determine the contents of cholalic acid and hyodeoxycholic acid in Qingkailing suppository by HPLC-ELSD（high performance liquid chromatography with evaporative light scattering detection） . METHODS： The analytical column was Diamonsil C18（250 mm × 4.6 mm, 5 μm） and the mobile phase consisted of 0.1% formic acidacetonitrile （gradient elution） with the temperature of the drift tube of the light scattering detector set at 110 ℃ and the flow rate of the nitrogen gas at 2.0 L·min^-1. RESULTS： The linear ranges of cholalic acid and hyodeoxycholic acid were 0.59-7.4μg（r = 0. 999 6） and 0.38- 4.8 μg（ r = 0. 999 7）, respectively, with their average recoveries at 99.20% （RSD = 1.4%, n = 6） and 98.57 % （RSD = 1.8%, n = 6）, respectively. CONCLUSION： The method is simple, accurate and well - separated, and it is applicable for the quality control of Qingkailing suppository.