Moreda-Piñeiro Antonio, Peña-Vázquez Elena, Hermelo-Herbello Paloma, Bermejo-Barrera Pilar, Moreda-Piñeiro Jorge, Alonso-Rodríguez Elia, Muniategui-Lorenzo Soledad, López-Mahía Purificación, Prada-Rodríguez Darío
Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n. 15782, Santiago de Compostela, Spain.
Anal Chem. 2008 Dec 1;80(23):9272-8. doi: 10.1021/ac801622u.
Matrix solid-phase dispersion (MSPD) has been applied to extract arsenical species (arsenite, As(III); arsenate, As(V); monomethylarsonic acid; dimethylarsinic acid, DMA; arsenobetaine, AsB; and arsenocholine) from seafood products. High-performance liquid chromatography coupled to inductively coupled plasma-mass spectrometry was used to separate and detect all arsenic species. Variables affecting MSPD, such as the solid support material (dispersing agent), solid support mass/sample mass ratio, elution solvent composition, and elution solvent volume, have been fully evaluated. Quantitative recoveries for inorganic and organic arsenic species have been obtained when using diatomaceous earth or octadecyl-functionalized silica gel (C18) as a solid support material, with a solid support mass/sample mass ratio of 7.0. Elution of arsenical compounds has been assessed using 10 mL of 50/50 methanol/ultrapure water as an elution solvent. The MSPD method has been found precise, with RSDs of approximately 9% for As(III), DMA, and As(V) and 3% for AsB. The developed procedure has been tested by analyzing different certified reference materials of marine origin such as DORM-2 and BCR 627, which offer certified contents for some arsenic species. The method has been also applied to assess arsenic speciation in different mollusks, cold water fishes, and white fishes.
基质固相分散萃取法(MSPD)已被应用于从海产品中提取砷的各种形态(亚砷酸盐,As(III);砷酸盐,As(V);一甲基胂酸;二甲基胂酸,DMA;砷甜菜碱,AsB;以及砷胆碱)。采用高效液相色谱与电感耦合等离子体质谱联用技术对所有砷形态进行分离和检测。已对影响MSPD的各种变量,如固体支持材料(分散剂)、固体支持材料质量/样品质量比、洗脱溶剂组成以及洗脱溶剂体积等进行了全面评估。当使用硅藻土或十八烷基官能化硅胶(C18)作为固体支持材料,且固体支持材料质量/样品质量比为7.0时,可实现无机和有机砷形态的定量回收。使用10 mL 50/50甲醇/超纯水作为洗脱溶剂对砷化合物进行洗脱。已发现MSPD方法具有良好的精密度,As(III)、DMA和As(V)的相对标准偏差约为9%,AsB的相对标准偏差为3%。通过分析不同的海洋来源有证标准物质,如DORM - 2和BCR 627(它们提供了某些砷形态的有证含量),对所开发的方法进行了测试。该方法还被应用于评估不同软体动物、冷水鱼和白鱼中的砷形态。