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[高效液相色谱法在磺胺类药物稳定性研究中的应用。3. 磺胺甲氧基嘧啶。水解分解产物的分离与鉴定]

[The use of high pressure liquid chromatography in stability studies of sulfonamides. 3. Sulfamethoxydiazine. Isolation and identification of hydrolytic decomposition products].

作者信息

Klimes J, Zahradnícek M

机构信息

Lehrstuhl für pharmazeutische Chemie, Pharmazeutische Fakultät der Karls-Universität, Hradec Kralové, CSSR.

出版信息

Pharmazie. 1987 Aug;42(8):511-3.

PMID:3432328
Abstract

The stability of sulphamethoxydiazine (1) in HCl (1 mol/l) under elevated temperature was investigated. Isolated decomposition products further served as standards for the selection of HPLC conditions. Three types of stationary phases were tested: Pragosil 5, MicroPak CN-10, MicroPak CH-10. The selection of mobile phases was made in such a way as to be able to inject 1 hydrolysate in HCl (1 mol/l) directly or after simple dilution. Detection was performed with an UV detector at the wavelength of 226 nm. A column packed with MicroPak CN-10 was selected to investigate the process of 1 decomposition. The method made it possible to quantify 1 in the course of hydrolysis and to illustrate the process of decomposition. On the basis of continuous examination of the development of decomposition products during the stability study it was possible to consider the chemism of the decomposition reaction.

摘要

研究了磺胺甲氧基嘧啶(1)在高温下于盐酸(1mol/L)中的稳定性。分离出的分解产物进一步用作选择高效液相色谱条件的标准物。测试了三种固定相:Pragosil 5、MicroPak CN - 10、MicroPak CH - 10。流动相的选择方式使得能够直接或在简单稀释后将1份盐酸(1mol/L)中的水解产物进样。使用紫外检测器在226nm波长下进行检测。选择填充有MicroPak CN - 10的色谱柱来研究1的分解过程。该方法能够在水解过程中对1进行定量,并阐明分解过程。基于在稳定性研究期间对分解产物生成情况的持续检测,得以考虑分解反应的化学机理。

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