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首页> 外文期刊>Journal of the Brazilian Chemical Society >Studies of zinc(II) in pharmaceutical and biological samples by extractive spectrophotometry: using pyridoxal-4-phenyl-3-thiosemicarbazone as chelating reagent
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Studies of zinc(II) in pharmaceutical and biological samples by extractive spectrophotometry: using pyridoxal-4-phenyl-3-thiosemicarbazone as chelating reagent

机译:萃取和分光光度法研究药物和生物样品中的锌(II):使用吡ido醛-4-苯基-3-硫代半乳糖胺作为螯合剂

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Pyridoxal-4-phenyl-3-thiosemicarbazone (PPT) is proposed as a new sensitive reagent for the sensitive extractive spectrophotometric determination of zinc(II). PPT reacts with zinc(II) in the pH range 5.0-6.0 to form a yellow colored complex, which was well extracted into n-butanol. The absorbance value of Zn(II)-PPT complex was measured at different intervals of time at 430 nm, to ascertain the stability of the complex. It was observed that the color development was instantaneous and stable for more than 48 h. The system obeyed Beer's law up to 6.0 μg mL-1 of zinc(II), with an excellent linearity in terms of correlation coefficient value of 0.999. The molar absorptivity and Sandell's sensitivity of the extracted species is 1.6 X 10(4) L mol-1 cm-1 and 4.085 X 10-3 μg cm-2 at 430 nm. The detection limit of the method is 0.04 μg mL-1. To assess precision of the method, determinations were carried out at different concentrations; the relative standard deviation does not exceed 3.1%. The composition of the zinc(II) complex with PPT was studied by the method of Job's continuous variation, molar ratio method, Asmus' method and slope ratio method. It has been satisfactorily applied for the determination of zinc(II), when present alone or in presence of diverse ions, which are usually associated with zinc(II) in pharmaceutical and biological samples. Various certified reference materials (NIST 1573, NBS 1572 and NIST SRM 8435) have been tested for the determination of zinc for evaluating the accuracy of the developed method. The results of the proposed method are in agreement with flame atomic absorption spectometry.
机译:提出了吡rid醛-4-苯基-3-硫代半脲(PPT)作为灵敏萃取光度法测定锌(II)的新型灵敏试剂。 PPT与pH在5.0-6.0范围内的锌(II)反应形成黄色络合物,将其充分萃取到正丁醇中。在不同的时间间隔在430 nm处测量Zn(II)-PPT配合物的吸光度值,以确定配合物的稳定性。观察到显色是瞬时的并且稳定超过48小时。该体系符合比尔定律,直到6.0μgmL-1的锌(II)都具有良好的线性,相关系数值为0.999。所提取物质的摩尔吸收率和Sandell敏感性在430 nm下为1.6 X 10(4)L mol-1 cm-1和4.085 X 10-3μgcm-2。该方法的检出限为0.04μgmL-1。为了评估该方法的精确度,在不同浓度下进行了测定。相对标准偏差不超过3.1%。采用Job连续变化法,摩尔比法,Asmus法和斜率法研究了PPT锌(II)配合物的组成。当单独存在或存在多种离子时,它已令人满意地用于测定锌(II),这些离子通常与药物和生物样品中的锌(II)有关。已测试了各种认证参考材料(NIST 1573,NBS 1572和NIST SRM 8435)来测定锌,以评估所开发方法的准确性。该方法的结果与火焰原子吸收光谱法相吻合。

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