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通过与1,2-萘醌-4-磺酸盐衍生化测定胶囊和血浆中盐酸金刚烷胺的选择性分光光度法和荧光分光光度法

Selective Spectrophotometric and Spectrofluorometric Methods for the Determination of Amantadine Hydrochloride in Capsules and Plasma via Derivatization with 1,2-Naphthoquinone-4-sulphonate.

作者信息

Mahmoud Ashraf M, Khalil Nasr Y, Darwish Ibrahim A, Aboul-Fadl Tarek

机构信息

Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P.O. Box 2457, Riyadh 11451, Saudi Arabia.

出版信息

Int J Anal Chem. 2009;2009:810104. doi: 10.1155/2009/810104. Epub 2009 Jan 25.

Abstract

New selective and sensitive spectrophotometric and spectrofluorometric methods have been developed and validated for the determination of amantadine hydrochloride (AMD) in capsules and plasma. The methods were based on the condensation of AMD with 1,2-naphthoquinone-4-sulphonate (NQS) in an alkaline medium to form an orange-colored product. The spectrophotometric method involved the measurement of the colored product at 460 nm. The spectrofluorometric method involved the reduction of the product with potassium borohydride, and the subsequent measurement of the formed fluorescent reduced AMD-NQS product at 382 nm after excitation at 293 nm. The variables that affected the reaction were carefully studied and optimized. Under the optimum conditions, linear relationships with good correlation coefficients (0.9972-0.9974) and low LOD (1.39 and 0.013 mug mL(-1)) were obtained in the ranges of 5-80 and 0.05-10 mug mL(-1) for the spectrophotometric and spectrofluorometric methods, respectively. The precisions of the methods were satisfactory; RSD </=2.04%. Both methods were successfully applied to the determination of AMD in capsules. As its higher sensitivity, the spectrofluorometric method was applied to the determination of AMD in plasma; the recovery was 96.3-101.2 +/- 0.57-4.2%. The results obtained by the proposed methods were comparable with those obtained by the official method.

摘要

已开发并验证了用于测定胶囊和血浆中盐酸金刚烷胺(AMD)的新型选择性和灵敏的分光光度法及荧光分光光度法。这些方法基于AMD在碱性介质中与1,2-萘醌-4-磺酸盐(NQS)缩合形成橙色产物。分光光度法涉及在460nm处测量有色产物。荧光分光光度法涉及用硼氢化钾还原产物,随后在293nm激发后于382nm处测量形成的荧光还原AMD-NQS产物。仔细研究并优化了影响反应的变量。在最佳条件下,分光光度法和荧光分光光度法分别在5 - 80和0.05 - 10μg mL⁻¹范围内获得了具有良好相关系数(0.9972 - 0.9974)和低检测限(1.39和0.013μg mL⁻¹)的线性关系。方法的精密度令人满意;相对标准偏差≤2.04%。两种方法均成功应用于胶囊中AMD的测定。由于其更高的灵敏度,荧光分光光度法应用于血浆中AMD的测定;回收率为96.3 - 101.2±0.57 - 4.2%。所提出方法获得的结果与官方方法获得的结果相当。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/b3cb/2814141/791b86f57e04/IJAC2009-810104.sch.001.jpg

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