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采用溴卤化和在线非极性固相萃取法测定藻类中的无机砷。

Determination of inorganic arsenic in algae using bromine halogenation and on-line nonpolar solid phase extraction followed by hydride generation atomic fluorescence spectrometry.

机构信息

Institute of Quality Standard and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, and Key Laboratory of Agro-food Safety and Quality, Ministry of Agriculture, Beijing 100081, China; Beijing Titan Instruments Company, Limited, Beijing 100015, China.

Institute of Quality Standard and Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, and Key Laboratory of Agro-food Safety and Quality, Ministry of Agriculture, Beijing 100081, China.

出版信息

Talanta. 2017 Aug 1;170:152-157. doi: 10.1016/j.talanta.2017.04.001. Epub 2017 Apr 4.

Abstract

Accurate, stable and fast analysis of toxic inorganic arsenic (iAs) in complicated and arsenosugar-rich algae matrix is always a challenge. Herein, a novel analytical method for iAs in algae was reported, using bromine halogenation and on-line nonpolar solid phase extraction (SPE) followed by hydride generation atomic fluorescence spectrometry (HG-AFS). The separation of iAs from algae was first performed by nonpolar SPE sorbent using Br for arsenic halogenation. Algae samples were extracted with 1% perchloric acid. Then, 1.5mL extract was reduced by 1% thiourea, and simultaneously reacted (for 30min) with 50μL of 10% KBr for converting iAs to AsBr after adding 3.5mL of 70% HCl to 5mL. A polystyrene (PS) resin cartridge was employed to retain arsenicals, which were hydrolyzed, eluted from the PS resin with HO, and categorized as iAs. The total iAs was quantified by HG-AFS. Under optimum conditions, the spiked recoveries of iAs in real algae samples were in the 82-96% range, and the method achieved a desirable limit of detection of 3μgkg. The inter-day relative standard deviations were 4.5% and 4.1% for spiked 100 and 500μgkg respectively, which proved acceptable for this method. For real algae samples analysis, the highest presence of iAs was found in sargassum fusiforme, followed by kelp, seaweed and laver.

摘要

准确、稳定、快速分析复杂且富含砷糖的藻类基质中的有毒无机砷(iAs)一直是一个挑战。本文报道了一种新的藻类中 iAs 分析方法,采用溴卤化和在线非极性固相萃取(SPE),随后进行氢化物发生原子荧光光谱法(HG-AFS)。首先,采用 Br 对藻类中的 iAs 进行非极性 SPE 分离,用 1%高氯酸提取藻类。然后,用 1%硫脲还原 1.5mL 提取物,同时在加入 3.5mL70%HCl 后与 50μL10%KBr 反应 30min,将 iAs 转化为 AsBr。采用聚苯乙烯(PS)树脂柱保留砷化合物,将其水解后,用 HO 洗脱 PS 树脂,并将其归类为 iAs。用 HG-AFS 定量测定总 iAs。在最佳条件下,真实藻类样品中 iAs 的加标回收率在 82-96%范围内,方法的检出限为 3μgkg。对于分别加标 100μgkg 和 500μgkg 的样品,日内相对标准偏差分别为 4.5%和 4.1%,这证明该方法具有良好的重现性。对于真实藻类样品分析,发现 iAs 含量最高的是马尾藻,其次是海带、海藻和紫菜。

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