Institute of Analytical Chemistry of the Czech Academy of Sciences, Veveří 97, 602 00, Brno, Czech Republic.
Matís, Research and Innovation, Vinlandsleid 12, 113, Reykjavik, Iceland.
Anal Chim Acta. 2019 Feb 21;1049:20-28. doi: 10.1016/j.aca.2018.11.036. Epub 2018 Nov 20.
It is advisable to monitor and regulate inorganic arsenic (iAs) in food and feedstuff. This work describes an update and validation of a method of selective hydride generation (HG) with inductively coupled plasma mass spectrometry (ICP-MS) for high-throughput screening of iAs content in seafood samples after microwave-assisted extraction with diluted nitric acid and hydrogen peroxide. High concentration of HCl (8 M) for HG along with hydrogen peroxide in samples of a same concentration as used for extraction leads to a selective conversion of iAs to volatile arsine that is released and transported to the detector. A minor contribution from methylarsonate (≈20% to iAs) was found, while HG from dimethylarsinate, trimethylarsine oxide is substantially suppressed (less than 1% to iAs). Methodology was applied to Certified Reference Materials (CRMs) TORT-3, DORM-3, DORM-4, DOLT-4, DOLT-5, PRON-1, SQID-1 and ERM-CE278k, in some of them iAs has been determined for the first time, and to various seaweed samples from a local store. The results were always compared with a reference method and selectivity of iAs determination was evaluated. An inter-laboratory reproducibility was tested by comparative analyses of six fish and four seaweed samples in three European laboratories, with good agreement of the results. The method of HG-ICP-MS is sensitive (limit of detection 2 μg kg iAs), well suited for screening of large number of samples and selective at iAs concentration levels at which maximum limits are expected to be set into EU legislation for marine samples.
建议对食品和饲料中的无机砷(iAs)进行监测和调控。本工作描述了一种更新和验证的方法,采用选择性氢化物发生(HG)与电感耦合等离子体质谱(ICP-MS),用于在微波辅助硝酸和过氧化氢提取后,对海鲜样品中的 iAs 含量进行高通量筛选。高浓度的 HCl(8 M)用于 HG 以及样品中与提取所用浓度相同的过氧化氢,导致 iAs 选择性转化为挥发性胂,然后释放并输送到检测器。发现甲基砷酸盐(≈iAs 的 20%)有少量贡献,而二甲基砷酸盐、三甲基氧化砷的 HG 则受到很大抑制(iAs 的不到 1%)。该方法应用于认证参考材料(CRMs) TORT-3、DORM-3、DORM-4、DOLT-4、DOLT-5、PRON-1、SQID-1 和 ERM-CE278k,其中一些材料是首次测定 iAs,还应用于当地商店的各种海藻样品。结果始终与参考方法进行比较,并评估了 iAs 测定的选择性。通过三个欧洲实验室对六个鱼类和四个海藻样本的比较分析,对实验室间的重现性进行了测试,结果具有良好的一致性。HG-ICP-MS 方法具有较高的灵敏度(iAs 的检测限为 2μg/kg),非常适合对大量样品进行筛选,并且在预计将在欧盟海洋样品法规中设定最大限量的 iAs 浓度水平下具有选择性。