2,2 -联吡啶试剂在纯乙酰半胱氨酸及其制剂分光光度测定中的应用

S. Hasan, S. Sultan
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引用次数: 0

摘要

本研究包括建立一种灵敏的分光光度法测定水溶液中乙酰半胱氨酸的方法。该方法是将乙酰半胱氨酸与铁离子氧化,生成的铁离子与2,2 -联吡啶反应形成粉红色配合物,该配合物稳定且可溶于水,在524 nm波长处吸收率最高。Beer定律的极限为乙酰半胱氨酸在20毫升(0.25-9.0µg)的终体积中浓度范围为(5-180)µg。摩尔吸光度为8633.28 L. mol -1 .cm -1,桑德尔敏感指数为0.0189µg。Cm -2。相对误差为-4.28% ~ 4.98%,相对标准偏差为±0.56% ~±3.75%。检出限(LOD)和定量限(LOQ)分别为0.01837和0.06124µg/ml,对常用药用辅料无影响。该方法与英国药典采用t检验的结果吻合良好(95%置信限),两者之间无显著差异。该方法可用于其制剂中乙酰半胱氨酸的测定。
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Utility of 2,2׳- Bipyridyl Reagent in Spectrophotometric Assay of Acetylcysteine in Pure Form and in Its Pharmaceutical Preparations
This study includes development of a sensitive spectrophotometric method for the determination of acetylcysteine in aqueous solution. The method is based on the oxidation of acetylcysteine with a ferric ion, followed by reacting of produced ferrous ion with 2,2 ׳ -bipyridyl to form a pink complex, which is stable and water-soluble and has the highest absorption at a wavelength of 524 nm. The limits of Beer's law were in the concentration range of (5-180) µg of acetylcysteine in a final volume of 20 milliliters (0.25-9.0 µg.ml -1 ) and the molar absorptivity of 8633.28 L. mol -1 .cm -1 , Sandell's sensitivity index of 0.0189 µg.cm -2 . The relative error of -4.28% – 4.98 % and relative standard deviation of ± 0.56% - ± 3.75% depending on the concentration level. The limit of detection limit(LOD) and limit of quantitation (LOQ) were calculated and equal to 0.01837 and 0.06124 µg/ml respectively, no inference was observed in the common pharmaceutical excipients. The results obtain by proposed method were in good agreement with those obtain from official British pharmacopoeia using t-test (at 95% confidence limit) which indicates that there is no significant differences between them. The method was successfully applied to determine acetylcysteine in its pharmaceutical preparations.
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审稿时长
24 weeks
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