甘氨胆酸中有关物质检查方法的研究  

Analysis of related substances in glycocholic acid

作　　者：冯文[1] 刘秀秀[1] 胡季[1] 晁若冰[1] 

机构地区：[1]四川大学华西药学院,成都610041

出　　处：《药物分析杂志》2014年第7期1200-1203,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的：建立HPLC-ELSD法测定甘氨胆酸的有关物质。方法：采用Gemini C18色谱柱（4.6 mm×150 mm,5μm）,以乙腈-0.1%甲酸（48∶52）为流动相,流速0.5 mL·min-1,ELSD检测,漂移管温度95℃,气体流速2.5 L·min-1,Gain为8。结果：在选定的条件下,甘氨胆酸与其中的5个杂质胆酸、甘氨胆酸乙酯、甘氨脱氧胆酸、甘氨脱氧胆酸乙酯、胆酸乙酯分离良好,它们的检测限相当的杂质浓度分别为0.008%、0.016%、0.016%、0.016%、0.022%、0.016%;5个杂质的平均回收率分别为100.5%、98.1%、105.7%、100.7%、101.4%;且上述6个物质浓度在3.75～31.25μg·mL-1范围内峰面积的对数与浓度的对数呈良好线性关系。结论：经方法学验证,本法简便、专属、准确,可用于甘氨胆酸中有关物质的检查。Objective： To establish an HPLC- ELSD method to determine the related substances in glycocholic acid. Methods： The HPLC method was performed on a Gemini C18column（ 4. 6 mm × 150 mm,5 μm） with the mobile phase of acetonitrile- 0. 1 % formic acid（ 48∶ 52）. The flow rate was 0. 5 mL·min- 1and the detector was Alltech ELSD 2000（ temperature of drift tube： 95 ℃; airflow velocity; 2. 5 L·min- 1; Gain： 8）. Results： Under this specific condition,glycocholic acid and its five impurities（ cholic acid,ethyl glycocholate,glycodeoxycholic acid,ethyl glycodeoxycholate,ethyl cholate） were well- separated. The limit of detection of glycocholic acid,cholic acid,ethyl glycocholate,glycodeoxycholic acid,ethyl glycodeoxycholate,ethyl cholate was 0. 008%,0. 016%,0. 016%,0. 016%,0. 022%,0. 016% respectively. The average recoveries of the five impurities were 100. 5%,98. 1%,105. 7%,100. 7%,101. 4%. Linearity was observed within the range of 3. 75- 31. 25 μg·mL- 1（ r 0. 9990） for all the analytes. Conclusion： The method was simple,specific,accurate and suitable for analyzing the related substances in glycocholic acid.

关 键 词：甘氨胆酸 胆酸 甘氨胆酸乙酯 甘氨脱氧胆酸 甘氨脱氧胆酸乙酯 胆酸乙酯 杂质 高效液相色谱法-蒸发光散色检测 方法验证 

分 类 号：R927[医药卫生—药学]