在长春胺存在其降解产物的情况下测定长春胺的稳定性指示方法。

Stability-indicating methods for determination of vincamine in presence of its degradation product.

作者信息

Shehata Mostafa A M, El Sayed Mohammad A, El Tarras Mohammad F, El Bardicy Mohammad G

机构信息

Department of Analytical Chemistry, Faculty of Pharmacy, Cairo University, Kasrel Aini Street, Cairo, Egypt ET 11562, Egypt.

出版信息

J Pharm Biomed Anal. 2005 Jun 1;38(1):72-8. doi: 10.1016/j.jpba.2004.11.057.

DOI:10.1016/j.jpba.2004.11.057

PMID:15907622

Abstract

Three different stability indicating assay methods are developed and validated for determination of vincamine in the presence of its degradation product (vincaminic acid). The first method is based on the derivative ratio zero crossing spectrophotometric technique using 0.1 N hydrochloric acid as a solvent. In the second method, measurements are based on spectro-densitometric technique using high performance thin-layer chromatography (HPTLC) plates with a developing system consisting of methanol-chloroform-ethyl acetate (2:1:1, v/v/v). The third method depends on high-performance liquid chromatography (HPLC). Separation of vincamine from vincaminic acid using Lichrocart RP-18 column (250 mm x 4.6 mm i.d.) with a mobile phase consisting of acetonitrile-ammonium carbonate (0.01 M) (7:3, v/v) is achieved. The methods showed high sensitivity with good linearity over the concentration ranges of 12 to 48 microg ml-1, 3 to 17 microg/spot, and 2 to 20 microg ml-1 for derivative spectrophotometry, spectro-densitometry and HPLC methods, respectively. The developed methods were successfully applied to the analysis of pharmaceutical formulations containing vincamine with excellent recoveries.

摘要

针对长春胺在其降解产物（长春胺酸）存在的情况下进行测定，开发并验证了三种不同的稳定性指示分析方法。第一种方法基于导数比零交叉分光光度技术，使用0.1 N盐酸作为溶剂。第二种方法基于分光密度测定技术，使用高效薄层色谱（HPTLC）板，展开系统由甲醇 - 氯仿 - 乙酸乙酯（2:1:1，v/v/v）组成。第三种方法依赖于高效液相色谱（HPLC）。使用Lichrocart RP - 18柱（250 mm×4.6 mm内径），以乙腈 - 碳酸铵（0.01 M）（7:3，v/v）作为流动相，实现了长春胺与长春胺酸的分离。对于导数分光光度法、分光密度测定法和HPLC法，这些方法在12至48 μg ml-1、3至17 μg/斑点和2至20 μg ml-1的浓度范围内分别显示出高灵敏度和良好的线性。所开发的方法成功应用于含有长春胺的药物制剂分析，回收率极佳。