酸水解-重氮偶联反应分光光度法测定尿中速尿及制剂。

H. Ali, Sumayha muhammed
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摘要

本文研究了用紫外分光光度法测定呋塞米(FUR)的方法,该方法是将呋塞米酸水解为游离的伯胺,重氮化,然后在碱性介质中与3,5 -二甲基苯酚(3,5 - dmph)偶联。在434 nm处测定吸光度,在0.4 ~ 50µg范围内符合比尔斯定律。moL-1的摩尔吸光度为1.3899 x104 L moL-1 .cm-1,灵敏度为0.0238x104µg。cm-2分别。对含有19种不同浓度FUR的溶液进行分析,相关系数为(0.9999),检出限、定量限分别为0.127、0.464µg。mL-1分别。用Job’s法对反应进行化学计量,摩尔比为1:1(重氮化FUR: 3,5 - dmph),并将该方法应用于合成尿液和药物配方中。加标尿液中FUR的回收率为(99±3.32)%,结果令人满意,并与现有的官方文献方法进行了比较。
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Use of Acidic Hydrolysis and Diazo Coupling Reaction for Spectrophotometric Determination of Furosemide in Urine and Pharmaceutical Formulation.
Simple and rapid spectrophotometric determination of furosemide (FUR) has been investigated .The method is based on acid hydrolysis of FUR to free primary aromatic amine and diazotization followed by coupling with 3, 5 di methyl phenol (3, 5-DMPH) at basic medium. The absorbance was measured at 434 nm, the method was optimized for best condition, and beers’ law is obeyed over the range of 0.4-50 µg.mL-1 with molar absorptivity and sandal’s sensitivity 1.3899 x104 L moL-1 .cm-1 and 0.0238x104 µg.cm-2 respectively. Analysis of solution containing nineteen different concentrations of FUR gave a correlation coefficient of (0.9999) and limit of detection, limit of quantitation were 0.127, 0.464µg.mL-1 respectively. The reaction stoichiometry was evaluated by Job’s and mole ratio method was found to be 1:1(diazotized FUR: 3, 5-DMPH) .The method was applied in synthetic urine and pharmaceutical formulation. The recovery of FUR in spiked urine was satisfactory resulting in the values of (99±3.32) %, the results of the suggested method was compared with available official literature method.
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