期刊
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
卷 53, 期 3, 页码 309-314出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jpba.2010.03.042
关键词
Acid halide; Acid chloride; 5-Chlorovaleroyl chloride; 4-Pentenoyl chloride; 4-Chlorovaleroyl chloride; 5-Chlorohexanoyl chloride; 4-Methyl-5-chlorovaleroyl chloride; 5-Chlorovaleric acid
5-Chlorovaleroyl chloride (5-CVC) is commonly used as an alkylating agent in the synthesis of pharmaceutical intermediates, active ingredients, as well as other specialty chemicals It is critical to monitor the impurities present in 5-CVC as they may have a direct impact on the impurity profile and quality of the final product. This paper describes the development and validation of a GC-FID method for the analysis of low level impurities of 5-CVC. This is the first method reported in the literature for the impurity determination of 5-CVC. The results of GC method development, with and without sample derivatization, are presented. The final method uses methanol for derivatization and separates methyl esters of 5-CVC and the key impurities, 4-pentenoyl chloride, 4-chlorovaleroyl chloride, 5-chlorohexanoyl chloride, and 4-methyl-5-chlorovaleroyl chloride 3-Methoxypyridine was used in the sample solvent to enable the detection of 5-chlorovaleric acid (5-CVA) which is the major degradant of 5-CVC The method was validated for specificity, linearity, accuracy, precision, sensitivity, and robustness This simple and robust GC approach may be applicable to impurity analysis of other acid chlorides or acid halides (C) 2010 Elsevier B V All rights reserved
作者
我是这篇论文的作者
点击您的名字以认领此论文并将其添加到您的个人资料中。
推荐
暂无数据