果糖嗪及脱氧果糖嗪首批国家对照品的研制  

A national reference standard for fructosazine and deoxyfructosazine

作　　者：刘博 郭云霄 张佟 黄露 贺兰英 范慧红 LIU Bo;GUO Yunxiao;ZHANG Tong;HUANG Lu;HE Lanying;FAN Huihong(Institute for Chemical Drug Control,National Institutes for Food and Drug Control,Beijing 102629,China;NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs,Beijing 102629,China;School of Pharmacy,China Pharmaceutical University,Nanjing Jiangsu 210009,China)

机构地区：[1]中国食品药品检定研究院化学药品检定所,北京102629 [2]国家药品监督管理局化学药品质量研究与评价重点实验室,北京102629 [3]中国药科大学药学院,江苏南京210009

出　　处：《中国药物警戒》2023年第3期282-285,291,共5页Chinese Journal of Pharmacovigilance

基　　金：北京市自然科学基金资助项目(7194337);中国食品药品检定研究院化学药品检定所重点实验室课题(1030050090142)。

摘　　要：目的为有效控制氨基葡萄糖类药物的产品质量,研制供氨基葡萄糖类药物原料及制剂有关物质检查用的果糖嗪及脱氧果糖嗪国家对照品。方法采用核磁共振、红外光谱、质谱手段进行结构鉴定,同时通过核磁共振氢谱与圆二色谱相结合的方式对2种待标品的绝对构型进行确认;采用2种高效液相色谱法进行纯度分析;分别利用多种分析方法对2种待标品的无机杂质、理化特性、均匀性与稳定性进行考察,采用质量平衡法进行含量赋值,并采用核磁共振定量法对赋值结果进行验证。结果2种杂质对照品结构准确,果糖嗪含量为98.0%,脱氧果糖嗪含量为95.1%。结论依据本研究所述方法研制的果糖嗪及脱氧果糖嗪首批国家对照品,可满足盐酸氨基葡萄糖、硫酸氨基葡萄糖原料及其制剂的质控需要。Objective To establish new national reference standards for fructosazine and deoxyfructosazine used for impurity determination of raw materials or preparations of glucosamine in order to ensure the quality of products of glucosamine.Methods UV,HRMS,1HNMR,13CNMR,2D NMR and CD were used to confirm the structure while the content of the product was calculated using the mass balance method before being verified by the QNMR method.Results The structure of this product was identified and the contents of fructosazine and deoxyfructosazine were assigned as 98.0%and 95.1%respectively.Conclusion Fructosazine and deoxyfructosazine have been established as national reference standards for the first time,which can be applied to quality control of glucosamine and related products.

关 键 词：果糖嗪 脱氧果糖嗪 氨基葡萄糖 研制对照品 

分 类 号：R927[医药卫生—药学]