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采用原子吸收光谱法检测生成取代胂的方法对婴儿食品中砷形态分析的样品制备。

Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection.

机构信息

Instituto Federal Sul-rio-grandense, Campus Pelotas, Praça Vinte de Setembro 455, Centro, 96015-360 Pelotas, RS, Brazil; Universidade Federal do Rio Grande do Sul, Instituto de Química, Av. Bento Gonçalves 9500, Agronomia, 91509-900 Porto Alegre, RS, Brazil; Institute of Analytical Chemistry of the CAS, v. v. i., Veveří 97, 602 00 Brno, Czech Republic.

Universidade Federal do Rio Grande do Sul, Instituto de Química, Av. Bento Gonçalves 9500, Agronomia, 91509-900 Porto Alegre, RS, Brazil.

出版信息

Talanta. 2017 Dec 1;175:406-412. doi: 10.1016/j.talanta.2017.07.055. Epub 2017 Jul 20.

Abstract

A slurry sampling procedure for arsenic speciation analysis in baby food by arsane generation, cryogenic trapping and detection with atomic absorption spectrometry is presented. Several procedures were tested for slurry preparation, including different reagents (HNO, HCl and tetramethylammonium hydroxide - TMAH) and their concentrations, water bath heating and ultrasound-assisted agitation. The best results for inorganic arsenic (iAs) and dimethylarsinate (DMA) were reached when using 3molL HCl under heating and ultrasound-assisted agitation. The developed method was applied for the analysis of five porridge powder and six baby meal samples. The trueness of the method was checked with a certified reference material (CRM) of total arsenic (tAs), iAs and DMA in rice (ERM-BC211). Arsenic recoveries (mass balance) for all samples and CRM were performed by the determination of the tAs by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted digestion and its comparison against the sum of the results from the speciation analysis. The relative limits of detection were 0.44, 0.24 and 0.16µgkg for iAs, methylarsonate and DMA, respectively. The concentrations of the most toxic arsenic species (iAs) in the analyzed baby food samples ranged between 4.2 and 99µgkg which were below the limits of 300, 200 and 100µgkg set by the Brazilian, Chinese and European legislation, respectively.

摘要

本文介绍了一种通过胂化生成、低温捕集和原子吸收光谱法检测,对婴儿食品中砷形态进行分析的泥浆取样程序。本文测试了几种泥浆制备程序,包括不同的试剂(HNO3、HCl 和四甲基氢氧化铵-TMAH)及其浓度、水浴加热和超声辅助搅拌。当使用 3molL HCl 加热和超声辅助搅拌时,对于无机砷(iAs)和二甲砷酸(DMA)的结果最佳。该方法应用于五种粥粉和六种婴儿餐样品的分析。采用总砷(tAs)、iAs 和 DMA 的认证参考物质(CRM)大米(ERM-BC211)检查方法的准确性。采用微波辅助消解后电感耦合等离子体质谱法(ICP-MS)测定 tAs,并将其与形态分析结果之和进行比较,对所有样品和 CRM 进行砷回收率(质量平衡)测定。对于 iAs、甲基砷酸和 DMA,相对检出限分别为 0.44、0.24 和 0.16μgkg。在分析的婴儿食品样品中,最有毒砷物种(iAs)的浓度范围在 4.2 到 99μgkg 之间,低于巴西、中国和欧洲法规分别设定的 300、200 和 100μgkg 限值。

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