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Combination of Ultrasonic-Assisted Cloud Point Extraction with Flame AAS for Preconcentration and Determination of Trace Amounts of Silver and Cadmium in Dried Nut and Vegetable Samples

机译:超声辅助浊点萃取-火焰原子吸收光谱法联合测定干果仁样品中的痕量银和镉

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In this article, ultrasonic-assisted cloud point extraction (UA-CPE) was used to the preconcentration of trace Ag(I) and Cd(II) in dried nut and vegetable samples. After ion association of Ag(I) and Cd(II) ions with 3,7-diamino-2,8-dimethyl-5-phenyl-phenaziniumchlorid (Safranin T) in the presence of excess potassium iodide (KI) at pH 6.0, the ternary complexes formed were quantitatively extracted into a micellar phase of poly(ethyleneglycol-mono-p-nonylphenylether) (PONPE 7.5) and then determined by flame atomic absorption spectrometry (FAAS). The matrix effects of possible some interfering ions on the method recovery and tolerance limits were also investigated. Under the optimized reagent conditions, the method was linearly dependent on the analyte concentrations in the range of 0.08-90 and 3-250 mu g L-1 with limits of detection of 0.02 and 0.9 mu g L-1 for Ag(I) and Cd(II), respectively. The reproducibility as the percent relative standard deviations (RSDs %) (0.5, 5.0, and 25 mu g L-1 for Ag(I) and 15, 30, and 100 mu g L-1 for Cd(II), n = 6) was lower than 3.6 % for both analytes. The accuracy of the method was controlled by analysis of two certified samples (SRM 1573a Tomato leaves and SRM 1643e Trace elements in waters) as well as recovery studies from spiked samples. It has been observed that the results obtained are in a good agreement with the certified values at confidence interval of 95 %. The method was successfully applied to determination of Ag(I) and Cd(II) in several dried nut and vegetable samples by FAAS after separation/preconcentration with UA-CPE.
机译:本文采用超声辅助浊点萃取(UA-CPE)对坚果和蔬菜样品中痕量的Ag(I)和Cd(II)进行了预浓缩。在pH值为6.0的过量碘化钾(KI)存在下,Ag(I)和Cd(II)离子与3,7-二氨基-2,8-二甲基-5-苯基-苯氮鎓氯化物(Safranin T)发生离子缔合后,将形成的三元复合物定量提取到聚乙二醇单对壬基苯基醚(PONPE 7.5)的胶束相中,然后通过火焰原子吸收光谱法(FAAS)测定。还研究了可能的某些干扰离子对方法回收率和公差极限的基质效应。在优化的试剂条件下,该方法线性依赖于0.08-90和3-250μg L-1范围内的分析物浓度,检测到的Ag(I)和L(g)的检测限为0.02和0.9μg L-1镉(II)。以相对标准偏差百分比(RSDs%)的重现性(对于Ag(I)为0.5、5.0和25μg L-1,对于Cd(II)为15、30和100μgL-1,n = 6两种分析物的)均低于3.6%。该方法的准确性通过分析两个认证样品(水中的SRM 1573a番茄叶和SRM 1643e微量元素)以及加标样品的回收率来控制。已经观察到,在95%的置信区间内,获得的结果与标准值非常吻合。该方法已成功应用于UA-CPE分离/预浓缩后,通过FAAS测定了一些干燥的坚果和蔬菜样品中的Ag(I)和Cd(II)。

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