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A Method Using Liquid-Liquid Microextraction in a Dynamic System for Preconcentration and Determination of Lead in Food Samples

机译:在动态系统中使用液微萃取技术进行食品中铅的预浓缩和测定的方法

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摘要

In this paper, a method using liquid-liquid microextraction in a dynamic system combined with spectrophotometry was developed for preconcentration and determination of lead in samples of shrimp and oyster. In the procedure, a system is proposed in which the organic drop is maintained at the bottom of a glass tube, with the passage of a stream of aqueous solution, avoiding the use of a microsyringe. The method is based on the transfer of metal species present in the aqueous phase in the form of complexes with the ligand 2-(5-bromo-2-pyridylazo)-5-dimethylaminophenol (5-Br-PADAP) to the organic phase trichloroethylene. Experimental conditions, such as sample flow rate, concentration of the complexing reagent, extraction solvent, time of extraction, and pH, were optimized. Under optimized conditions, the limit of detection and quantification obtained were 0.48 and 1.60 mu g L-1, respectively. The accuracy was evaluated by the determination of lead in the certified reference material BCR-414, Plankton. The procedure was applied to the determination of lead in samples of shellfish, with recoveries ranging from 92 to 103 %. The method enabled a fast, accurate, and simple alternative for the determination of lead in seafood samples.
机译:本文开发了一种在动态系统中使用液-液微萃取结合分光光度法的方法,用于虾和牡蛎样品中铅的富集和测定。在该方法中,提出了一种系统,其中有机液滴保持在玻璃管的底部,同时使水溶液流通过,从而避免使用微注射器。该方法基于与配体2-(5-溴-2-吡啶基偶氮)-5-二甲基氨基苯酚(5-Br-PADAP)形成配合物形式存在于水相中的金属物质转移到有机相三氯乙烯中。优化了实验条件,例如样品流速,络合剂浓度,萃取溶剂,萃取时间和pH。在最佳条件下,检测限和定量限分别为0.48和1.60μg L-1。通过确定浮游生物认证的参考材料BCR-414中的铅来评估准确性。该方法用于测定贝类样品中的铅,回收率在92%至103%之间。该方法为测定海鲜样品中的铅提供了一种快速,准确和简单的替代方法。

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