摘要
目的为加强对抗溃疡药薁磺酸钠原料药的质量控制,合成了其中可能存在的两个有关物质并鉴定其结构。方法以愈创薁为起始原料,经发烟硫酸磺化制得薁磺酸钠原料中的有关物质1和有关物质2与1的混合物;有关物质1的化学结构经MS、NMR谱确证,采用LC-MS法对混合物中有关物质2的结构进行分析。结果与结论确定了有关物质1的结构为1,4-二甲基-7-异丙基薁-2-磺酸钠(1);有关物质2为薁磺酸钠的同分异构体,推测其结构为4-甲基-7-异丙基-1-薁甲基磺酸钠(2)。有关物质1和1与2的混合物可作为薁磺酸钠原料药质量控制的杂质对照品。
To improve the quality control of guaiazulene sulfonate sodium, two impurities were synthesized and identified. Using guaiazulene as the starting material, impurity 1 as well as the mixture of impurity 2 and 1 were obtained respectively by sulfonation with oleuna, The structure of impurity 1 was confirmed via MS and NMR,and the structure of impurity 2 was comfirmed via LC-MS. The impurity 1 was identified as sodium 1,4-dimethyl-7-isopropylazulene-2-sulfonate （1）. Impurity 2 was the isomer of guaiazulene sulfonate sodium, the structure of which is deemed to be sodium 4-methyl-7-isopropyl-1-azulene-methanesulfonate （2）. The two impurities can be used as the related substances in the quality control of guaiazulene sulfonate sodium.
出处
《中国药物化学杂志》
CAS
CSCD
2016年第1期41-44,共4页
Chinese Journal of Medicinal Chemistry
关键词
薁磺酸钠
有关物质
磺化
同分异构体
ezetimibe
cholesterol absorption inhibitor
process improvement
