气相色谱法测定片剂中的硝酸异山梨酯

Gas-liquid chromatographic determination of isosorbide dinitrate in tablets.

作者信息

Prue D G, Johnson R N, Kho B T

出版信息

J Assoc Off Anal Chem. 1977 Nov;60(6):1341-4.

Abstract

A gas-liquid chromatographic (GLC) method is described for determining isosorbide dinitrate (ISDN) in tablets. ISDN is extracted from tablet excipients by a 2-phase system composed of water-ethyl ether, and detected and quantitated with a flame ionization detector after separation from the internal standard (glyceryl tributyrate) on a 3% OV-210 column. Ten replicate assays on 2 different batches of tablets, each containing 5 mg ISDN, gave coefficients of variation of 1.16 and 1.48%, respectively. Comparison of results obtained for tablets containing 5, 10, and 40 mg ISDN, and for diluted isosorbide dinitrate raw material containing 25% ISDN, showed good correlation among the GLC, USP colorimetric, and USP polarographic procedures. Assay of synthetic mixtures containing ISDN, isosorbide-2-mononitrate, and isosorbide-5-mononitrate demonstrated that the GLC procedure is specific for ISDN, whereas the USP polarographic procedure is subject to interference from the mononitrates.

摘要

本文描述了一种用于测定片剂中硝酸异山梨酯（ISDN）的气液色谱（GLC）方法。ISDN通过由水 - 乙醚组成的两相系统从片剂辅料中萃取出来，并在3% OV - 210柱上与内标（三丁酸甘油酯）分离后，用火焰离子化检测器进行检测和定量。对2个不同批次、每片含5 mg ISDN的片剂进行10次重复测定，变异系数分别为1.16%和1.48%。对含5、10和40 mg ISDN的片剂以及含25% ISDN的稀释硝酸异山梨酯原料所获得的结果进行比较，结果表明GLC、美国药典比色法和美国药典极谱法之间具有良好的相关性。对含有ISDN、2 - 单硝酸异山梨酯和5 - 单硝酸异山梨酯的合成混合物进行分析表明，GLC方法对ISDN具有特异性，而美国药典极谱法会受到单硝酸盐的干扰。