高效阴离子交换-脉冲安培法分析藻酸双酯钠的单糖组成和比例  

Analysis of monosaccharide composition and monosaccharide ratio in propylene glycol alginate sodium sulphate drugs by high performance anion exchange chromatograghy-pulsed amperometric detection

作　　者：王悦[1,2] 陈欣桐 李振华 宋玉娟 范慧红[1,2] WANG Yue;CHEN Xin-tong;LI Zhen-hua;SONG Yu-juan;FAN Hui-hong(National Institute for Food and Drug Control,Beijing 102629,China;NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,北京102629 [2]化学药品质量研究与评价重点实验室,北京102629

出　　处：《药学学报》2021年第9期2346-2351,共6页Acta Pharmaceutica Sinica

基　　金：国家重大新药创制课题资助项目(2015ZX09303001);海洋药物国家重点实验室开放性课题资助项目(LMDBKF201806)。

摘　　要：藻酸双酯钠为类肝素药物,临床上主要用于治疗缺血性心、脑血管疾病,本研究建立藻酸双酯钠的单糖组成和单糖比例测定方法。通过正交分析的方法确定了样品前处理最佳反应条件,样品经过三氟乙酸水解,氢氧化钠溶液中和,采用高效阴离子交换-脉冲安培检测法,使用CarboPac?PA20阴离子交换柱分离,流动相采用200 mmol·L^(-1)氢氧化钠溶液和1 mol·L^(-1)醋酸钠溶液梯度洗脱,采用脉冲安培检测器,金工作电极, Ag/AgCl参比电极进行检测。对方法的线性、准确度和精密度进行了考察,结果表明该方法具有简单、专属、灵敏、应用范围广等特点。对不同企业藻酸双酯钠原料药进行了测定,能够准确测定藻酸双酯钠单糖组成,为藻酸双酯钠的结构鉴定提供单糖信息。The paper aims to establish the method to determine the monosaccharide composition and monosaccharide ratio in propylene glycol alginate sodium sulphate(PSS). Samples were hydrolyzed with trifluoroacetic acid, neutralized with sodium hydroxide solution after the reaction conditions for sample pretreatment were optimized via orthogonal analysis. A high performance anion exchange chromatograghy(HPAEC) coupled with pulsed amperometric detector(PAD) was performed on a CarboPac?PA20, using 200 mmol·L^(-1) sodium hydroxide solution and 1 mol·L^(-1) sodium acetate solution as mobile phase. The established HPAEC-PAD method was validated by testing the linear relationship, precision and accuracy, and showed exclusive, sensitive, rapid and wide use. The monosaccharide composition of PSS from different manufacture can be accurately determined with great significance for the structural identification of PSS.

关 键 词：阴离子交换 脉冲安培法 糖组成 藻酸双酯钠 甘露糖醛酸 古罗糖醛酸 

分 类 号：R917[医药卫生—药物分析学]