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通过与4-氯-7-硝基苯并-2-恶唑-1,3-二氮杂茂衍生化,用荧光分光光度法测定剂型和血浆中的氟伏沙明。

Spectrofluorimetric determination of fluvoxamine in dosage forms and plasma via derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole.

作者信息

Darwish Ibrahim A, Amer Sawsan M, Abdine Heba H, Al-Rayes Lama I

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

J Fluoresc. 2009 May;19(3):463-71. doi: 10.1007/s10895-008-0433-z. Epub 2008 Oct 23.

DOI:10.1007/s10895-008-0433-z
PMID:18949539
Abstract

A highly sensitive and simple spectrofluorimetric method has been developed and validated for the determination of the antidepressant fluvoxamine (FXM) in its dosage forms and plasma. The method was based on nucleophilic substitution reaction of FXM with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole in an alkaline medium (pH 8) to form a highly fluorescent derivative that was measured at 535 nm after excitation at 470 nm. The factors affecting the reaction was carefully studied and optimized. The kinetics of the reaction was investigated, and the reaction mechanism was presented. Under the optimized conditions, linear relationship with good correlation coefficient (0.9995) was found between the fluorescence intensity and FXM concentration in the range of 65-800 ng ml(-1). The limits of detection and quantitation for the method were 21 and 64 ng ml(-1), respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 2.17%. The proposed method was successfully applied to the determination of FXM in its pharmaceutical tablets with good accuracy; the recovery values were 97.8-101.4 +/- 1.08-2.75%. The results obtained by the proposed method were comparable with those obtained by the official method. The high sensitivity of the method allowed its successful application to the analysis of FXM in spiked human plasma. The proposed method is superior to the previously reported spectrofluorimetric method for determination of FXM in terms of its simplicity. The proposed method is practical and valuable for its routine application in quality control and clinical laboratories for analysis of FXM.

摘要

已开发并验证了一种高灵敏度且简单的荧光分光光度法,用于测定抗抑郁药氟伏沙明(FXM)的剂型及血浆中的含量。该方法基于FXM在碱性介质(pH 8)中与4-氯-7-硝基苯并-2-恶唑-1,3-二氮杂茂的亲核取代反应,形成一种高荧光衍生物,在470 nm激发后于535 nm处进行测定。仔细研究并优化了影响该反应的因素。研究了反应动力学,并提出了反应机理。在优化条件下,荧光强度与FXM浓度在65 - 800 ng ml⁻¹范围内呈良好的线性关系,相关系数为0.9995。该方法的检测限和定量限分别为21和64 ng ml⁻¹。方法的精密度令人满意;相对标准偏差值不超过2.17%。所提出的方法成功应用于药物片剂中FXM的测定,准确度良好;回收率为97.8 - 101.4 ± 1.08 - 2.75%。所提方法得到的结果与官方方法得到的结果具有可比性。该方法的高灵敏度使其成功应用于加标人血浆中FXM的分析。所提方法在简便性方面优于先前报道的用于测定FXM的荧光分光光度法。所提方法对于在质量控制和临床实验室中常规分析FXM具有实用性和价值。

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