Ulu Sevgi Tatar, Aydogmus Zeynep
Department of Analytical Chemistry, Faculty of Pharmacy, Istanbul University, Istanbul, Turkey.
Chem Pharm Bull (Tokyo). 2008 Dec;56(12):1635-8. doi: 10.1248/cpb.56.1635.
A new rapid and sensitive procedure assay is proposed for the spectrophotometric determination of tianeptine. The developed method involves formation of colored chloroform extractable ion-pair complexes of tianeptine with bromophenol blue (BPB), bromocresol green (BCG), bromothymol blue (BTB) and methyl orange (MO) in acidic medium. Beer's law is obeyed in the concentration ranges 3.0-12.0, 4.0-16.0, 4.0-14.0 and 2.0-10.0 microg ml(-1) with BPB, BCG, BTB and MO, respectively. The detection limit of tianeptine was found to be 1.8 microg ml(-1) for BPB, 2.0 for BCG, 2.0 microg ml(-1) for BTB and 1.0 microg ml(-1) for MO. Validation of the method was performed in terms of linearity, limit of detection (LOD), quantification (LOQ), accuracy and precision. Common excipients used as additives in pharmaceutical preparations do not interfere in the proposed method. The proposed method has been applied to determination of the examined drugs in pharmaceutical formulations and the results demonstrated that the method is equally accurate, precise, and reproducible as the official method. The t-test showed no significant difference at 95% confidence level.
提出了一种用于分光光度法测定噻奈普汀的快速灵敏的新方法。所开发的方法包括在酸性介质中，噻奈普汀与溴酚蓝（BPB）、溴甲酚绿（BCG）、溴百里酚蓝（BTB）和甲基橙（MO）形成可被氯仿萃取的有色离子对络合物。分别在3.0 - 12.0、4.0 - 16.0、4.0 - 14.0和2.0 - 10.0 μg ml⁻¹的浓度范围内，BPB、BCG、BTB和MO符合比尔定律。发现噻奈普汀对BPB的检测限为1.8 μg ml⁻¹，对BCG为2.0，对BTB为2.0 μg ml⁻¹，对MO为1.0 μg ml⁻¹。该方法在线性、检测限（LOD）、定量限（LOQ）、准确度和精密度方面进行了验证。药物制剂中用作添加剂的常见辅料在所提出的方法中不产生干扰。所提出的方法已应用于药物制剂中被测药物的测定，结果表明该方法与官方方法同样准确、精密且可重现。t检验表明在95%置信水平下无显著差异。
