HPLC方法分析工业5-氨基酮戊酸盐酸盐杂质  

Analysis of impurities of crude 5-aminolevulinic acid hydrochloride by HPLC

作　　者：李海春[1] 高赛男[1] 蒋蕾[1] 彭海生[1] LI Hai-chun GAO Sai-nan JIANG Lei PENG Hai-sheng(Department of Pharmaceutics,Daqing Branch,Harbin Medical Universit)

机构地区：[1]哈尔滨医科大学(大庆)药学院,黑龙江大庆163319

出　　处：《哈尔滨商业大学学报（自然科学版）》2016年第4期429-432,共4页Journal of Harbin University of Commerce：Natural Sciences Edition

基　　金：黑龙江省自然科学基金项目(D201031;ZD201613);哈尔滨医科大学大庆校区优秀硕士生导师基金;哈尔滨医科大学于维汉院士杰出青年培养基金;哈尔滨医科大学研究生创新基金(YJSCX2015-60HYD);黑龙江省普通本科高等学校青年创新人才培养计划项目(UNPYSCT-2015036)

摘　　要：建立HPLC法测定5-氨基酮戊酸（5-ALA）盐酸盐粗品中的杂质百分含量.使用带有DAD检测器的安捷伦高效液相色谱仪进行检测,色谱柱为岛津Inertsil ODS-SP色谱柱（4.6 mm×250mm,5μm）;流动相为离子对溶液（辛烷磺酸钠2.16 g、磷酸二氢钠3.12 g,加水配成1 000 m L溶液,磷酸调节p H值为3.65）-乙腈（82∶18）;柱温30℃;流速1 m L/min;波长205 nm;线性范围0.2～1.0mg/m L之间,R2=0.999 2,回收率为104%,RSD为0.96%,方法能将主峰与杂质峰有效分离,可作为5-ALA盐酸盐杂质百分含量分析方法.A HPLC method to analyze the impurities of crude 5- aminolevulinic acid（ 5-ALA） samples was established. HPLC analysis was performed with Agilent liquid chromatograph equipped with DAD detector. An Inertsil ODS- SP analytical column（ 4. 6 mm × 250 mm,5 μm） was used to separate the samples. The mobile phase was the mixture of acetonitrile and ion pair solution（ 18 ∶ 82）. Sodium octane sulfonate of 2. 16 g and monosodium phosphate of 3. 12 g were dissolved into 1 000 m L water,and then the p H value of solution was regulated to 3. 65 to be used as ion pair solution. The detection wavelength was 205 nm and the column temperature was kept at 30 ℃. The linear relationship was between 0. 2 and1. 0 mg / m L（ R2= 0. 999 2）. The average recoveries of 5- ALA was 104%（ RSD = 0.96%）. The protocol was able to separate all the compositions of crude 5- ALA,monitoring the purity of 5- ALA.

关 键 词：5-氨基酮戊酸盐酸盐 高效液相色谱法 辛烷磺酸钠 杂质 

分 类 号：TQ463[化学工程—制药化工]