胆酸钠原料中有机溶剂残留的研究

Research of residual solvents in crude sodium cholate

为建立气相色谱-氢火焰离子化检测法(GC-FID)定量测定胆酸钠原料中乙醇、乙醚溶剂残留的新方法,将胆酸钠用乙腈提取,采用HP-INNOWax气相毛细管柱分离,以氮气为载气,流速为1.5mL·min^-1,使用氢火焰离子化检测器进行检测,进样口温度为200℃,检测器温度为250℃.结果表明:胆酸钠原料中乙醇、乙醚的百分含量分别为0.7,0.9,0.6mg·g^-1和30,40,30μg·g^-1,按《中国药典》规定,均处于正常范围内.此方法简便易操作,重现性好,可适用于胆酸钠原料药中残留溶剂的研究和检测.

In order to establish a new method for the quantitative determination of residual solvents(ethanol and ether)in sodium cholate by gas chromatography equipped with flame ionization detector(GC-FID),sodium cholate was extracted by acetonitrile and separated on HP-INNO Wax column by using nitrogen as the carrier gas(1.5 mL·min^-1),with the detector temperature at 250℃and the injection port temperature at 200℃.The results indicated that the contents of ethanol and ether in several crude sodium cholate samples were 0.7,0.9,0.6 mg·g^-1 and 30,40,30μg·g^-1 respectively,which was within the specified range according to“Chinese Pharmacopeia”.This method is simple,easy to operate,and reproducible,which can be applied to the study and detection of residual solvents in crude sodium cholate.