胆酸钠原料中有机溶剂残留的研究
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摘要
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-INNO Wax气相毛细管柱分离,以氮气为载气,流速为1.5 m L·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0.7,0.9,0.6 mg·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 m L · 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 30,40,30 μg·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.
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 m L · 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 30,40,30 μg·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.
引文
[1]汪祺,何轶,郑笑为,等.牛磺胆酸钠对照品标定方法的建立[J].中国现代中药,2016,18(10):1279-1284.
[2]朱强,石朝周,孙汉清.牛磺胆酸钠的合成及其药理作用[J].中国药学杂志,1997,32(4):236-238.
[3]公瑞煜,张达,吕志良,等.牛磺鹅去氧胆酸钠的提取及与鹅去氧胆酸钠的药理作用比较[J].精细化工,2007,24(10):975-978.
[4]石志辉,徐麟皓,周锐.牛磺熊去氧胆酸钠抑制小鼠间歇性低氧模型肺组织中内质网应激的激活[J].中南大学学报(医学版),2015,40(11):1165-1172.
[5]中华人民共和国卫生部药典委员会.中华人民共和国卫生部药品标准[S].二部第六册.北京:中华人民共和国卫生部药典委员会,1998:98.
[6]梁爽,洪松,汤峥,等.生物表面活性剂胆酸钠对氯酚的增溶[J].环境化学,2017,36(2):345-355.
[7]贾霖,黄国清,王宝维,等.鹅胆汁中鹅脱氧胆酸和胆红素提取工艺研究[J].食品工业科技,2012,33(9):292-294.
[8]Kumar K,Patial B S,Chauhan S.Conductivity and fluorescence studies on the micellization properties of sodium cholate and sodium deoxycholate in aqueous medium at different temperatures:Effect of selected amino acids[J].J Chem Thermodyn,2015,82:25-33.
[9]邓旭坤,吴非,陈旅翼,等.气相色谱法分析大麻药多糖成分中单糖组成[J].中南民族大学学报(自然科学版),2015,34(2):48-51.
[2]朱强,石朝周,孙汉清.牛磺胆酸钠的合成及其药理作用[J].中国药学杂志,1997,32(4):236-238.
[3]公瑞煜,张达,吕志良,等.牛磺鹅去氧胆酸钠的提取及与鹅去氧胆酸钠的药理作用比较[J].精细化工,2007,24(10):975-978.
[4]石志辉,徐麟皓,周锐.牛磺熊去氧胆酸钠抑制小鼠间歇性低氧模型肺组织中内质网应激的激活[J].中南大学学报(医学版),2015,40(11):1165-1172.
[5]中华人民共和国卫生部药典委员会.中华人民共和国卫生部药品标准[S].二部第六册.北京:中华人民共和国卫生部药典委员会,1998:98.
[6]梁爽,洪松,汤峥,等.生物表面活性剂胆酸钠对氯酚的增溶[J].环境化学,2017,36(2):345-355.
[7]贾霖,黄国清,王宝维,等.鹅胆汁中鹅脱氧胆酸和胆红素提取工艺研究[J].食品工业科技,2012,33(9):292-294.
[8]Kumar K,Patial B S,Chauhan S.Conductivity and fluorescence studies on the micellization properties of sodium cholate and sodium deoxycholate in aqueous medium at different temperatures:Effect of selected amino acids[J].J Chem Thermodyn,2015,82:25-33.
[9]邓旭坤,吴非,陈旅翼,等.气相色谱法分析大麻药多糖成分中单糖组成[J].中南民族大学学报(自然科学版),2015,34(2):48-51.