Faculty of Chemistry, Division of Analytical Chemistry and Chemical Metallurgy, Wroclaw University of Science and Technology , Wroclaw, Poland.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2021 Feb;38(2):280-292. doi: 10.1080/19440049.2020.1852318. Epub 2021 Jan 6.
A strategy was developed for the determination of total As in birch saps (BSs) by hydride generation (HG) coupled with inductively coupled plasma optical emission spectrometry (ICP-OES). We proposed and validated a simple and robust HG-ICP-OES method with no need for tedious and long sample preparation before measurements. Corresponding As hydride was generated in reaction with NaBH (1.0%) in acidic conditions (10 mol L HCl) after pre-reduction of As(V) to As(III) in a KI (0.5%)-ascorbic acid (2.0%)-HCl (3 mol L) mixture. Several different sample preparation procedures, including digestive and non-digestive approaches, were tested in order to improve the detectability of As using HG-ICP-OES. Reactivity of As towards HG under conditions of a real sample was investigated to check potential interfering effects coming from undecomposed sample matrix constituents. The proposed method included the direct analysis of untreated samples (only pre-reduction prior to HG) and precision (<6% as relative standard deviation), accuracy (94.7-108.7% as recoveries) and sensitivity (limit of detection at 0.26 ng mL) that was suitable for trace analysis. An absence of matrix effects allowed external calibration for quantification of As. Applicability of the method was demonstrated by determination of As in several commercially available bottled BSs.
本研究开发了一种利用氢化物发生(HG)与电感耦合等离子体光学发射光谱法(ICP-OES)联用测定桦树汁(BSs)中总砷的策略。我们提出并验证了一种简单而稳健的 HG-ICP-OES 方法,无需在测量前进行繁琐且冗长的样品制备。在 KI(0.5%)-抗坏血酸(2.0%)-HCl(3 mol L)混合溶液中将 As(V)预还原为 As(III)后,在酸性条件下(10 mol L HCl),用 1.0%的 NaBH 与样品反应生成相应的砷氢化物。为了提高 HG-ICP-OES 检测砷的灵敏度,我们测试了几种不同的样品制备程序,包括消化和非消化方法。考察了实际样品中 As 对 HG 的反应性,以检查来自未分解样品基质成分的潜在干扰影响。该方法包括对未经处理的样品(仅在 HG 之前进行预还原)进行直接分析,其具有良好的精密度(相对标准偏差<6%)、准确性(回收率为 94.7-108.7%)和灵敏度(检测限为 0.26 ng mL),适用于痕量分析。不存在基质效应允许进行外部校准以定量测定砷。该方法通过测定几种市售瓶装 BSs 中的砷,证明了其适用性。