【摘要】 建立巴洛合成母液中3-甲胺基哌啶盐酸盐的分离、分析测定方法。根据样品中各组分溶解性差异,采用了柱层析分离的方法。中性Al2O3层析柱,用丙酮淋洗出试样中的有机杂质,再用甲醇钠-甲醇溶液淋洗,分离出母液中3-甲胺基哌啶盐酸盐。用气相色谱法进行测定:采用毛细管柱,固定液为OV-101,90～240℃程序升温,苯甲酸甲酯为内标物,测定3-甲胺基哌啶盐酸盐的含量,平均含量2.43%,准确度98%,精密度0.02。所建立的方法简单、快速、重复性好,结果准确,精密度好。更多还原

【Abstract】 A separate and analysis method for measure content of 3-methyla minopiperidin HCl salt in balofloxacin synthesis mother liquid was developed.According to every component different solubility,neuter Al2O3 column laminar analysis separate method was used.Organic impurity would be elute out by CH3COCH3.Then 3-methyla minopiperidin HCl salt would be completely elute out by CH3ONa-CH3OH.The 3-methyla minopiperidin HCl salt were measurated by gas chromatograph capillary column,90～240 ℃ temperature programmed,internal standard: C6H5COOCH3,stationary liquid: OV-101,the average content was 2.43 %,accuracy was 98 %,precision was 0.02.The method was simple,quick and accurate with good reproducibiliy.更多还原