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作 者:金剑炜 俞春晓[1,2] 于绪平 章良[1,2] 宋少奇 梁玲玲 王士琦 肖群艳[1] 徐晓攀 吴春雷 JIN Jian-wei;YU Chun-xiao;YU Xu-ping;ZHANG Liang;SONG Shao-qi;LIANG Ling-ling;WANG Shi-qi;XIAO Qun-yan;XU Xiao-pan;WU Chun-lei(Zhejiang Pharmaceutical Co.Ltd.,Shaoxing 312000,China;Zhejiang Engineering Research Center of Fat-soluble Vitamin,Shaoxing 312000,China;College of Chemeal Engineering,Shaoxing University,Shaoxing 312000,China)
机构地区:[1]浙江医药股份有限公司,浙江绍兴312000 [2]脂溶性维生素浙江省工程研究中心,浙江绍兴312000 [3]绍兴文理学院化学化工学院,浙江绍兴312000
出 处:《安徽化工》2025年第1期100-103,共4页Anhui Chemical Industry
摘 要:采用普通柱层析方法从胆固醇母液中分离得到一个杂质,通过质谱与核磁进行结构分析,并乙酯化后与相关标准物进行比对,确证该杂质结构为7-酮基胆固醇,这为胆固醇的质量研究提供了杂质对照品。以分离得到的7-酮基胆固醇为原料,经乙酸酐在3号位酯化定量得到3-醋酸酐胆固醇,再与对甲苯磺酰肼反应生成相应的腙,接着在NaH作用下脱去腙得到3-醋酸酐-7-脱氢胆固醇,最后在氢氧化钠作用下水解得到7-脱氢胆固醇,总收率约为69.6%。An important oxidation product from cholesterol as well as impurity,was isolated from the mother liquor of cholesterol using column chromatography.The structure of the impurity was identified as 7-oxo-cholesterol based on the analysis of its MS and NMR data,and further confirmed with reference to the literature data.This provides impurity reference standards for the quality research of cholesterol.using the above 7-oxo-cholesterol-3-acetate as the raw material as follows:7-oxo-cholesterol-3-acetate reacted with p-toluenesulfonyl hydrazide to afford the corresponding hydrazone,then removal the hydrazone in the presence of NaH to afford 7-dehydrocholesterol-3-acetate,the target product 7-dehydrocholesterol obtained via a hydrolysis in the presence of NaOH.The overall yield was about 69.6%.
关 键 词:胆固醇 7-酮基胆固醇 7-脱氢胆固醇 杂质 分离纯化
分 类 号:R917[医药卫生—药物分析学]
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