固相萃取分离-电感耦合等离子体质谱(ICP-MS)法测定海产品中的无机砷

Determination of Inorganic Arsenic in Seafood by Inductively Coupled Plasma Mass Spectrometry with Solid Phase Extraction

分别将N-(β氨乙基)-γ-氨丙基三甲氧基硅烷(AEAPTMS)、3-巯丙基三甲氧基硅烷(MPTMS)与四乙氧基硅烷(TEOS)水解共聚,制备氨基\巯基键合的硅胶材料。将此材料作为固相萃取(SPE)小柱的填充材料,建立了固相萃取快速分离富集海产品样品中五价砷As(Ⅴ)和三价砷As(Ⅲ),电感耦合等离子体质谱(ICP-MS)法测定海产品中无机砷的方法。研究了固相萃取小柱对无机砷的吸附原理、性能和洗脱条件,在pH=3~4范围内固相萃取小柱材料有良好的选择吸附性,利用硝酸(2%)可将As(Ⅴ)洗脱,利用硝酸(2%)+KIO3(0.1mol/L)可将As(Ⅲ)洗脱。实际样品检测的加标回收率在72.3%~102%,实现了海产品样品中无机砷形态快速、方便、准确的检测。

N-(βaminoethyl)-γ-aminopropyltrimethoxysilane(AEAPTMS)and 3-Mercaptopropyltrimethoxysilane(MPTMS)was added to tetraethoxysilane(TEOS)mixture respectively to get amino\sulfhydryl bonded silica gel materials.This material is used as the filling material of SPE column.The method for the determination of inorganic arsenic in marine products by inductively coupled plasma mass spectrometry(ICP-MS)with solid phase extraction was established.Adsorption principle,adsorption performance and elution conditions of solid phase extraction column for inorganic arsenic were studied,and the results show that this solid phase extraction column material has good selective adsorption capacity in the range of pH=3-4,As(V)can be eluted with 2% nitric acid,As(Ⅲ)can be eluted with 2% nitric acid and 0.1 mol/L KIO3 mixed solution.The standard addition recovery of the actual sample is between 72.3% and 102%,the method has realized the rapid,convenient and accurate detection of inorganic arsenic in seafood samples.