Determination and Speciation of Selenium in Pharmaceutical Samples, Spiked Veterinary Drug Samples with a Kinetic Catalytic Method

E. Bağda
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Abstract

In the present study a new kinetic catalytic method was developed for the sensitive determination of selenium in pharmaceutical formulations. The reaction between basic blue 3 (BB3) and sulphide catalysed by Se (IV) in the presence of acetic-phosphoric-boric acid buffer system. The decrease in the absorbance at 654 nm indicated the reduction of BB3. The presence of selenium (IV) accelerated the reaction rate. The method based on the linear correlation between amount of Se(IV) and reaction rate. Under optimum conditions, the linear calibration range was found as 0.1-2.0 µg ml-1 by the fixed time method for the 0.5-5 min. The tolerance limits of various species was also studied. The interfering effect of some cations such as Cr3+, Fe3+, and Hg2+ was reduced with using cation exchange resin. The proposed method was successfully applied to spiked nasal spray and veterinary drug samples. Besides, total selenium, Se (IV) and Se (VI) speciation also conducted with reducing Se (VI) to Se (IV) with HCl in the synthetic mixtures.
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动力学催化法测定兽药样品中硒的含量及形态
本文建立了一种新的动力学催化法,用于药物制剂中硒的灵敏测定。在醋酸-磷酸-硼酸缓冲体系存在下,用Se (IV)催化碱性蓝3 (BB3)与硫化物的反应。654 nm处吸光度下降表明BB3减少。硒(IV)的存在加快了反应速度。该方法基于Se(IV)的量与反应速率的线性关系。在最佳条件下,采用固定时间法,在0.5 ~ 5 min的时间内,线性校准范围为0.1 ~ 2.0µg ml-1。使用阳离子交换树脂可降低Cr3+、Fe3+、Hg2+等阳离子的干扰作用。该方法成功地应用于加标鼻喷雾剂和兽药样品中。此外,在合成混合物中,用盐酸将Se (VI)还原为Se (IV),总硒、Se (IV)和Se (VI)形态也发生了变化。
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