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通过离子对络合物形成对纯吡罗昔康、胶囊和人血清样品进行灵敏且选择性的分光光度测定。

Sensitive and selective spectrophotometric assay of piroxicam in pure form, capsule and human blood serum samples via ion-pair complex formation.

作者信息

Alizadeh Nina, Keyhanian Fereshteh

机构信息

Department of Chemistry, Faculty of Science, University of Guilan, Namjoo Street, P.B. 41335-1914, Rasht, Iran.

Department of Chemistry, Faculty of Science, University of Guilan, Namjoo Street, P.B. 41335-1914, Rasht, Iran.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2014 Sep 15;130:238-44. doi: 10.1016/j.saa.2014.03.074. Epub 2014 Apr 2.

Abstract

A simple, accurate and highly sensitive spectrophotometric method has been developed for the rapid determination of piroxicam (PX) in pure and pharmaceutical formulations. The proposed method involves formation of stable yellow colored ion-pair complexes of the amino derivative (basic nitrogen) of PX with three sulphonphthalein acid dyes namely; bromocresol green (BCG), bromothymol blue (BTB), bromophenol blue (BPB) in acidic medium. The colored species exhibited absorption maxima at 438, 429 and 432 nm with molar absorptivity values of 9.400×10(3), 1.218×10(3) and 1.02×10(4) L mol(-1) cm(-1) for PX-BCG, PX-BTB and PX-BPB complexes, respectively. The effect of optimum conditions via acidity, reagent concentration, time and solvent were studied. The reactions were extremely rapid at room temperature and the absorbance values remained constant for 48h. Beer's law was obeyed with a good correlation coefficient in the concentration ranges 1-100 μg mL(-1) for BCG, BTB complexes and 1-95 μg mL(-1) for BPB complex. The composition ratio of the ion-pair complexes were found to be 1:1 in all cases as established by Job's method. No interference was observed from common additives and excipients which may be present in the pharmaceutical preparations. The proposed method was successfully applied for the determination of PX in capsule and human blood serum samples with good accuracy and precision.

摘要

已开发出一种简单、准确且高度灵敏的分光光度法,用于快速测定纯品及药物制剂中的吡罗昔康(PX)。该方法包括在酸性介质中,使PX的氨基衍生物(碱性氮)与三种磺酞酸染料,即溴甲酚绿(BCG)、溴百里酚蓝(BTB)、溴酚蓝(BPB)形成稳定的黄色离子对络合物。这些有色物质在438、429和432nm处呈现吸收最大值,对于PX - BCG、PX - BTB和PX - BPB络合物,其摩尔吸光系数分别为9.400×10(3)、1.218×10(3)和1.02×10(4) L mol(-1) cm(-1)。研究了酸度、试剂浓度、时间和溶剂等最佳条件的影响。反应在室温下极快,吸光度值在48小时内保持恒定。对于BCG、BTB络合物,在1 - 100μg mL(-1)浓度范围内,以及对于BPB络合物在1 - 95μg mL(-1)浓度范围内,符合比尔定律且相关系数良好。通过乔布法确定,在所有情况下离子对络合物的组成比均为1:1。未观察到药物制剂中可能存在的常见添加剂和辅料的干扰。所提出的方法成功应用于胶囊和人血清样品中PX的测定,具有良好的准确度和精密度。

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