Cava-Montesinos Patricia, Nilles Katja, Cervera M Luisa, Guardia Miguel de la
Department of Analytical Chemistry, Faculty of Chemistry, University of Valencia, 50 Dr. Moliner Street, 46100 Burjassot, Valencia, Spain.
Talanta. 2005 May 15;66(4):895-901. doi: 10.1016/j.talanta.2004.12.042. Epub 2005 Jan 25.
A rapid, sensitive and economic method has been developed for the direct determination of toxic species of arsenic present in fish and mussel samples. As(III), As(V), dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) were determined by hydride generation-atomic fluorescence spectrometry using a series of proportional equations without the need of a chromatographic previous separation. The method is based on the extraction of arsenic species from fish through sonication with HNO(3) 3moll(-1) and 0.1% (m/v) Triton and washing of the solid phase with 0.1% (m/v) EDTA, followed by direct measurement of the corresponding hydrides in four different experimental conditions. The limit of detection of the method was 0.62ngg(-1) for As(III), 2.1ngg(-1) for As(V), 1.8ngg(-1) for MMA and 5.4ngg(-1) for DMA, in all cases expressed in terms of sample dry weight. The mean relative standard deviation values (R.S.D.) in actual sample analysis were: 6.8% for As(III), 10.3% for As(V), 8.5% for MMA and 7.4% for DMA at concentration levels from 0.08mgkg(-1) As(III) to 1.3mgkg(-1) DMA. Recovery studies provided percentages greater than 93% for all species in spiked samples. The analysis of SRM DORM-2 and CRM 627 certified materials evidenced that the method is suitable for the accurate determination of arsenic species in fish.
已开发出一种快速、灵敏且经济的方法,用于直接测定鱼类和贻贝样品中存在的有毒砷物种。采用一系列比例方程,通过氢化物发生-原子荧光光谱法测定As(III)、As(V)、二甲基砷酸(DMA)和一甲基砷酸(MMA),无需预先进行色谱分离。该方法基于以下步骤:用3mol/L的HNO₃和0.1%(m/v)的 Triton对鱼进行超声处理以提取砷物种,并用0.1%(m/v)的EDTA洗涤固相,然后在四种不同实验条件下直接测量相应的氢化物。该方法的检测限为:As(III)为0.62ng/g,As(V)为2.1ng/g,MMA为1.8ng/g,DMA为5.4ng/g,所有情况均以样品干重表示。在实际样品分析中,平均相对标准偏差值(R.S.D.)为:在0.08mg/kg As(III)至1.3mg/kg DMA的浓度水平下,As(III)为6.8%,As(V)为10.3%,MMA为8.5%,DMA为7.4%。加标样品的回收率研究表明,所有物种的回收率均大于93%。对SRM DORM-2和CRM 627认证材料的分析证明,该方法适用于准确测定鱼类中的砷物种。