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青霉素中N,N - 二甲基苯胺的气相色谱法测定

GLC determination of N,N-dimethylaniline in penicillins.

作者信息

Margosis M

出版信息

J Pharm Sci. 1977 Nov;66(11):1634-6. doi: 10.1002/jps.2600661136.

Abstract

A reliable GLC procedure was developed for the determination of residual N,N-dimethylaniline as a contaminant in ampicillin commerical samples from various sources. The procedure was similarly applied to other penicillins and cephalosporins. The method involves dissolution of the sample in aqueous alkali, extraction of the organic base with cyclohexane containing naphthalene as an internal standard, and injection into gas chromatograph with a phenyl methyl silicone column. Levels of 0.1 ppm of dimethylaniline were easily measured with a coefficient of variation less than 10%, and recoveries from spiked samples exceeded 99%.

摘要

开发了一种可靠的气相色谱法,用于测定来自不同来源的氨苄青霉素商业样品中作为污染物的残留N,N-二甲基苯胺。该方法同样适用于其他青霉素和头孢菌素。该方法包括将样品溶解在碱水溶液中,用含有萘作为内标的环己烷萃取有机碱,然后注入配备苯基甲基硅氧烷柱的气相色谱仪中。0.1 ppm的二甲基苯胺水平很容易测量,变异系数小于10%,加标样品的回收率超过99%。

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