文章摘要
刘文举.磺胺二甲嘧啶-对羟基苯甲酸共晶在乙腈溶剂中的三元相图测定[J].精细化工,2020,37(9):
磺胺二甲嘧啶-对羟基苯甲酸共晶在乙腈溶剂中的三元相图测定
Determination of ternary phase diagram of sulfamethazine-p-hydroxybenzoic acid cocrystal in acetonitrile solvent
投稿时间:2020-03-04  修订日期:2020-04-19
DOI:
中文关键词: 磺胺二甲嘧啶  对羟基苯甲酸  高效液相色谱  三元相图  共晶
英文关键词: sulfadimidine  p-hydroxybenzoic acid  HPLC  ternary phase diagram  cocrystal
基金项目:河南省科技攻关,河南工业大学科技创新人才培育计划
作者单位E-mail
刘文举 河南工业大学 wenjuliu@haut.edu.cn 
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中文摘要:
      建立一种HPLC同时分析测定溶液中磺胺二甲嘧啶和对羟基苯甲酸含量的方法,结果表明以乙腈-磷酸水溶液(pH=3.15)为流动相,体积比为18∶82时,能使磺胺二甲嘧啶和对羟基苯甲酸在9 min内迅速分离,该分析方法精密性和稳定性的RSD值均小于2%,磺胺二甲嘧啶和对羟基苯甲酸的平均回收率分别为98.73%、98.90% 。在此基础上,采用溶液法制备磺胺二甲嘧啶-对羟基苯甲酸共晶,在298.15K、303.15K时,建立共晶体在乙腈溶剂中的三元相图。采用XRD、DSC、SEM对磺胺二甲嘧啶、对羟基苯甲酸和在298.15K时部分干燥固相进行表征分析。结果表明,磺胺二甲嘧啶-对羟基苯甲酸-乙腈体系相图是对称相图,随着温度的升高,磺胺二甲嘧啶-对羟基苯甲酸共晶区域增大,有利于共晶的形成。
英文摘要:
      A HPLC method was developed for the simultaneous analysis and determination of sulfamethazine and p-hydroxybenzoic acid in solution. The results showed that when acetonitrile-phosphoric acid aqueous solution (pH = 3.15) was used as the mobile phase and the volume ratio was 18∶82, sulfamethazine and p-hydroxybenzoic acid were quickly separated in 9 minutes. The RSD values of precision and stability of the method are less than 2%. The average recoveries of sulfamethazine and p-hydroxybenzoic acid are 98.73% and 98.90%, respectively. On this basis, the sulfamethazine-p-hydroxybenzoic acid cocrystal was prepared by the solution method. At 298.15K and 303.15K, the ternary phase diagram of the cocrystal in acetonitrile solvent was established. The XRD, DSC, and SEM were used to characterize the sulfamethazine and p-hydroxybenzoic acid and the partially dried solid phase at 298.15K. The results show that the phase diagram of the sulfamethazine-p-hydroxybenzoic acid-acetonitrile system is a symmetrical phase diagram. As the temperature increases, the sulfamethazine-p-hydroxybenzoic acid cocrystal region increases, which is conducive to the formation of the cocrystal .
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