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用法比浊法测定头孢克肟

Determination of cefixime in pure form, in pharmaceutical products and biological samples through fluorescence quenching of eosin Y.

机构信息

Department of Chemistry, Bacha Khan University Charsadda, Pakistan.

出版信息

Luminescence. 2021 Mar;36(2):515-524. doi: 10.1002/bio.3971. Epub 2020 Nov 18.

Abstract

A simple, economic and validated spectrofluorimetric method was developed to assay cefixime (CFX). The technique relies on the quenching effect of CFX on the fluorescence intensity of eosin Y in the presence of acetate buffer pH 3.4 to produce an ion-pair complex that is measured at 549 nm using an excitation wavelength of 300 nm. Reaction-influencing factors were carefully investigated and optimized. The fluorescence quenching value was linear to the CFX concentration in the range 0.2-40 μg/ml with a correlation coefficient of 0.992. The calculated limit of detection and limit of quantification were found to be 0.00242 and 0.0080 μg ml , respectively. The selectivity of the method was confirmed by studying the effects of excipients and no interference was distinguished. The developed method was used to determine CFX in marketable products and in biological samples. To validate the method, directives of the International Conference on Harmonization were applied and per cent recoveries obtained ranged from 95.30 to 102.50% for pharmaceutical products and from 97.00 to 103.00% for biological fluids.

摘要

建立了一种简单、经济且经过验证的分光荧光法来测定头孢克肟(CFX)。该技术依赖于 CFX 在醋酸盐缓冲液 pH 3.4 存在下对曙红 Y 荧光强度的猝灭效应,以产生离子对复合物,然后在 300nm 的激发波长下在 549nm 处测量。仔细研究并优化了反应影响因素。荧光猝灭值与 CFX 浓度在 0.2-40μg/ml 范围内呈线性关系,相关系数为 0.992。计算得到的检测限和定量限分别为 0.00242 和 0.0080μg/ml。通过研究赋形剂的影响证实了该方法的选择性,未观察到干扰。该方法用于测定市售产品和生物样品中的 CFX。为了验证该方法,应用了国际协调会议的指导原则,对于药物产品,回收率在 95.30%至 102.50%之间,对于生物体液,回收率在 97.00%至 103.00%之间。

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