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比色法和分光光度法测定吐根及其制剂中的总生物碱和非酚性生物碱。

Colorimetric and spectrophotometric determination of total and non-phenolic alkaloids in ipeca and its formulations.

作者信息

Saleh M R, El-Masry S, El-Shaer N

出版信息

J Assoc Off Anal Chem. 1979 Sep;62(5):1113-5.

PMID:43328
Abstract

A simple method, requiring no chromatographic separation, is presented for the determination of the total and non-phenolic alkaloids in ipeca and its preparations. The complex formed between the alkaloid and methyl orange at pH 5.0 is extracted with chloroform and treated with 0.1N NaOH. The liberated dye, determined at 460 nm, is a measure of the total alkaloids. The chloroform phase remaining is treated with 0.1N H2SO4, and the acid extract is measured at 283 nm for the non-phenolic alkaloids, calculated as emetine. The proposed method was successfully applied to samples of ipeca powder, ipeca tincture, and 3 British Pharmaceutical Codex mixtures containing ipeca tincture, namely, ipecacuanha mixture, pediatric; ipecacuanha and ammonia mixture, pediatric; and belladonna and ipecacuanha mixture, pediatric. The proposed method compares favorably with the Egyptian Pharmacopoeia, British Pharmacopoeia, and USP methods and has a relative standard deviation of 1.54%. The present procedure is less time-consuming and requires about 45 and 90 min for the assay of ipeca tincture and powder, respectively. Only a small sample (0.2 mL tincture of 1.0 g powder) is required.

摘要

本文介绍了一种无需色谱分离的简单方法,用于测定吐根及其制剂中的总生物碱和非酚性生物碱。在pH 5.0条件下,生物碱与甲基橙形成的络合物用氯仿萃取,并用0.1N氢氧化钠处理。在460nm处测定释放出的染料,以此作为总生物碱的量度。剩余的氯仿相用0.1N硫酸处理,酸萃取液在283nm处测定非酚性生物碱,以吐根碱计算。该方法成功应用于吐根粉、吐根酊以及3种含吐根酊的英国药典混合物样品,即小儿吐根合剂、小儿吐根和氨合剂、小儿颠茄和吐根合剂。该方法与埃及药典、英国药典和美国药典方法相比具有优势,相对标准偏差为1.54%。本方法耗时较少,测定吐根酊和吐根粉分别约需45分钟和90分钟。仅需少量样品(1.0g粉末的0.2mL酊剂)。

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