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优化和验证分光荧光光度法测定药物制剂中头孢羟氨苄和头孢呋辛钠的含量。

Optimization and validation of spectrofluorimetric method for determination of cefadroxile and cefuroxime sodium in pharmaceutical formulations.

机构信息

Chemistry Department, Faculty of Science, University of Khartoum, PO Box 321, Khartoum 11115, Sudan.

出版信息

Luminescence. 2013 Jul-Aug;28(4):490-5. doi: 10.1002/bio.2481. Epub 2013 Jan 24.

Abstract

A simple, accurate, precise and validated spectrofluorimetric method is proposed for the determination of two cephalosporins, namely, cefadroxile (cefa) and cefuroxime sodium (cefu) in pharmaceutical formulations. The method is based on a reaction between cephalosporins with 1,2-naphthoquinone-4-sulfonate in alkaline medium, to form fluorescent derivatives that are extracted with chloroform and subsequently measured at 610 and 605 nm after excitation at 470 and 460 nm for cefa and cefu respectively. The optimum experimental conditions have been studied. Beer's law is obeyed over the concentrations of 20-70 ng/mL and 15-40 ng/mL for cefa and cefu, respectively. The detection limits were 4.46 ng/mL and 3.02 ng/mL with a linear regression correlation coefficient of 0.9984 and 0.998, and recoveries ranging 97.50-109.96% and 95.73-98.89% for cefa and cefu, respectively. The effects of pH, temperature, reaction time, 1,2-naphthoquinone-4-sulfonic concentration and extraction solvent on the determination of cefa and cefu, have been examined. The proposed method can be applied for the determination of cefa and cefu in pharmaceutical formulations in quality control laboratories.

摘要

提出了一种简单、准确、精密和经过验证的荧光分光光度法,用于测定两种头孢菌素,即头孢羟氨苄(cefadroxile,cefa)和头孢呋辛钠(cefuroxime sodium,cefu)在药物制剂中的含量。该方法基于头孢菌素与 1,2-萘醌-4-磺酸盐在碱性介质中的反应,形成荧光衍生物,用氯仿萃取,然后分别在 470nm 和 460nm 激发下,在 610nm 和 605nm 处测量。优化了实验条件。cefadroxile 和 cefuroxime 的浓度在 20-70ng/mL 和 15-40ng/mL 范围内符合比尔定律。检测限分别为 4.46ng/mL 和 3.02ng/mL,线性回归相关系数分别为 0.9984 和 0.998,cefadroxile 和 cefuroxime 的回收率分别为 97.50%-109.96%和 95.73%-98.89%。考察了 pH 值、温度、反应时间、1,2-萘醌-4-磺酸钠浓度和萃取溶剂对 cefa 和 cefu 测定的影响。该方法可用于药物制剂中 cefa 和 cefu 的质量控制实验室测定。

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