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利用米拉贝隆对乙酰氧基汞荧光素试剂的猝灭作用测定米拉贝隆的经验证的荧光分光光度法。

Validated spectrofluorimetric method for determination of mirabegron by utilizing its quenching effect on acetoxymercuric fluorescein reagent.

作者信息

Morshedy S, Omran G, Abdullatef O A, Omar M, Talaat W

机构信息

Faculty of Pharmacy, Damnhour University, Damnhour, Egypt.

Faculty of Pharmacy, Pharos University, Smoha, Alexandria, Egypt.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2020 Oct 5;239:118509. doi: 10.1016/j.saa.2020.118509. Epub 2020 May 20.

Abstract

A reliable, sensitive, simple and inexpensive spectrofluorimetric method has been developed for assay of mirabegron in bulk powder and in its tablets. The method depends on the quenching effect of mirabegron on the fluorescence intensity of acetoxymercuric fluorescein (AMF) reagent at ƛem of 520 nm and ƛex of 498 nm. Parameters that may affect the reaction such as pH, AMF solution concentration, temperature, time and diluting solvents were studied and optimized. Under the optimized conditions, the proposed method was applied over the concentration range of 1-5 μg mL with acceptable linearity (r = 0.9997). The developed method was validated according to ICH guidelines in terms of accuracy, precision, linearity, range, LOD and LOQ. The proposed method was applied to analyze mirabegron in Bladogra® 50 mg tablets with acceptable recovery% of 100.41 and RSD% of 1.72. The results obtained were compared to those obtained by a previously reported TLC method.

摘要

已开发出一种可靠、灵敏、简单且廉价的荧光分光光度法,用于测定米拉贝隆原料药及其片剂中的含量。该方法基于米拉贝隆对乙酰氧基汞荧光素(AMF)试剂在发射波长520 nm和激发波长498 nm处荧光强度的猝灭作用。研究并优化了可能影响反应的参数,如pH值、AMF溶液浓度、温度、时间和稀释溶剂。在优化条件下,该方法在1 - 5 μg mL的浓度范围内应用,线性良好(r = 0.9997)。所开发的方法按照国际协调会议(ICH)指南在准确度、精密度、线性、范围、检测限和定量限方面进行了验证。该方法应用于分析Bladogra® 50 mg片剂中的米拉贝隆,回收率为100.41%,相对标准偏差为1.72%,结果令人满意。将所得结果与先前报道的薄层色谱法所得结果进行了比较。

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