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氟伏沙明与1,2-萘醌-4-磺酸盐反应的分光光度研究:动力学、反应机理及在其剂型中测定氟伏沙明的应用

Spectrophotometric study for the reaction between fluvoxamine and 1,2-naphthoquinone-4-sulphonate: Kinetic, mechanism and use for determination of fluvoxamine in its dosage forms.

作者信息

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

机构信息

Department of Pharmaceutical Chemistry, King Saud University, Riyadh, Saudi Arabia.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2009 May;72(4):897-902. doi: 10.1016/j.saa.2008.12.009. Epub 2008 Dec 24.

Abstract

Spectrophotometric study was carried out, for the first time, to investigate the reaction between the antidepressant fluvoxamine (FXM) and 1,2-naphthoquinone-4-sulphonate (NQS) reagent. In alkaline medium (pH 9), an orange-colored product exhibiting maximum absorption peak (lambda(max)) at 470nm was produced. The kinetics of the reaction was investigated and its activation energy was found to be 2.65kcalmol(-1). Because of this low activation energy, the reaction proceeded easily. The stoichiometry of the reaction was determined and the reaction mechanism was postulated. This color-developing reaction was successfully employed in the development of simple and rapid spectrophotometric method for determination of FXM in its pharmaceutical dosage forms. Under the optimized reaction conditions, Beer's law correlating the absorbance (A) with FXM concentration (C) was obeyed in the range of 0.6-8microgml(-1). The regression equation for the calibration data was A=0.0086+0.1348C, with good correlation coefficient (0.9996). The molar absorptivity (epsilon) was 5.9x10(4)lmol(-1)cm(-1). The limits of detection and quantification were 0.2 and 0.6microgml(-1), respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 2%. The proposed method was successfully applied to the determination of FXM in its pharmaceutical tablets with good accuracy and precisions; the label claim percentage was 100.47+/-0.96%. The results obtained by the proposed method were comparable with those obtained by the official method. The proposed method is superior to all the previously reported spectrophotometric methods for determination of FXM in terms of its simplicity and sensitivity. The method is practical and valuable for its routine application in quality control laboratories for analysis of FXM.

摘要

首次进行了分光光度法研究,以考察抗抑郁药氟伏沙明(FXM)与1,2-萘醌-4-磺酸盐(NQS)试剂之间的反应。在碱性介质(pH 9)中,生成了一种在470nm处呈现最大吸收峰(λ(max))的橙色产物。研究了该反应的动力学,发现其活化能为2.65kcal/mol(-1)。由于该活化能较低,反应易于进行。确定了反应的化学计量关系并推测了反应机理。这种显色反应成功地用于开发一种简单快速的分光光度法,用于测定其药物剂型中的FXM。在优化的反应条件下,吸光度(A)与FXM浓度(C)的比尔定律在0.6 - 8μg/ml(-1)范围内成立。校准数据的回归方程为A = 0.0086 + 0.1348C,相关系数良好(0.9996)。摩尔吸光系数(ε)为5.9×10(4)l/mol(-1)cm(-1)。检测限和定量限分别为0.2和0.6μg/ml(-1)。该方法的精密度令人满意;相对标准偏差值不超过2%。所提出的方法成功地应用于其药物片剂中FXM的测定,具有良好的准确度和精密度;标示量百分率为100.47±0.96%。所提出的方法得到的结果与官方方法得到的结果相当。所提出的方法在简单性和灵敏度方面优于所有先前报道的分光光度法测定FXM的方法。该方法对于在质量控制实验室中常规应用于FXM分析具有实用性和价值。

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