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Pre-concentration procedure for determination of copper and zinc in food samples by sequential multi-element flame atomic absorption spectrometry

机译:连续多元素火焰原子吸收光谱法测定食品样品中铜和锌的预富集程序

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In this paper is proposed a simultaneous pre-concentration procedure using cloud point extraction for the determination of copper and zinc in food samples employing sequential multi-element flame atomic absorption spectrometry (FS-FAAS). The reagent used is 1-(2-pyridylazo)-2-naphthol (PAN) and the micellar phase is obtained using the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) and centrifugation. The optimization step was performed using Box-Behnken design for three factors: solution pH, reagent concentration and buffer concentration. A multiple response function was established in order to get an experimental condition for simultaneous extraction of copper and zinc. Under the optimized experimental conditions, the method allows the determination of copper with a limit of detection (3 sigma(b)/S, LOD) of 0.1 mu gL(-1), precision expressed as relative standard deviation (R.S.D.) of 2.1 and 1.3% (N=10), for copper concentrations of 10 and 50 wg L-1, respectively. Zinc is determined with a LOD of 0.15 mu g L-1 and precision as R.S.D. of 2.7 and 1.7% for concentrations of 10 and 50 wg L-1, respectively. The enhancement factors obtained were 36 and 32 for copper and zinc, respectively. The accuracy was assessed by analysis of certified reference materials, namely. SRM 1567a - Wheat Flour and SRM 8433 - Corn Bran from National Institute of Standards & Technology and BCR 189-wholemeal flour from Institute of Reference Materials and Measurements. The method was applied to the determination of copper and zinc in oats, powdered chocolate, corn flour and wheat flour samples. The copper content in the samples analyzed varied from 1.14 to 3.28 mu g g(-1) and zinc from 8.7 to 22.9 mu g g(-1). (C) 2008 Elsevier B.V. All rights reserved.
机译:本文提出了一种使用浊点萃取的同时预富集程序,采用顺序多元素火焰原子吸收光谱法(FS-FAAS)测定食品中的铜和锌。所使用的试剂是1-(2-吡啶基偶氮)-2-萘酚(PAN),并且使用非离子表面活性剂辛基苯氧基聚乙氧基乙醇(Triton X-114)并离心获得胶束相。使用Box-Behnken设计针对三个因素执行优化步骤:溶液pH,试剂浓度和缓冲液浓度。建立了多重响应函数,以便获得同时提取铜和锌的实验条件。在优化的实验条件下,该方法允许以0.1μgL(-1)的检出限(3 sigma(b)/ S,LOD)测定铜,精密度表示为2.1的相对标准偏差(RSD),铜浓度分别为10和50 wg L-1时为1.3%(N = 10)。锌的LOD为0.15μg L-1,精密度为R.S.D.浓度分别为10和50 wg L-1时分别为2.7和1.7%。铜和锌的增强因子分别为36和32。准确度是通过对认证参考材料进行分析来评估的。 SRM 1567a-小麦粉和SRM 8433-美国国家标准技术研究院的玉米麸皮和来自参考材料与测量学会的BCR 189全麦粉。该方法用于测定燕麦,巧克力粉,玉米粉和小麦粉样品中的铜和锌。分析样品中的铜含量为1.14至3.28微克g(-1),锌为8.7至22.9微克g(-1)。 (C)2008 Elsevier B.V.保留所有权利。

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