高效液相色谱-电感耦合等离子体质谱联用测定牡蛎中的有机锡

摘要

采用微波辅助萃取结合高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)法测定牡蛎样品中的有机锡.用含有1.0 mol/L冰醋酸和0.5 mol/L醋酸钠的甲醇溶液作为萃取溶剂,在微波功率60 W条件下萃取牡蛎样品20 min,样品经过滤后采用HPLC-ICP-MS法进行分析检测.在优化的条件下,二丁基锡、三丁基锡和三苯基锡3种有机锡的加标回收率分别为104%、99.3%和113%,检出限分别为0.33、0.22、0.48ng/g.并采用CE 477贻贝标准物质进行方法验证,该方法的测定值与标准值符合.%Organotins in oyster samples were determined by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) after microwaveassisted extraction.Oyster samples were extracted under the conditions of microwave power 60 W for 20 min, while 1.0 mol/L acetic acid and 0.5 mol/L sodium acetate in methanol severed as extraction solvent.After filtration, samples were determined by HPLC-ICP-MS.Under the optimized conditions, the recoveries of dibutyltin, tributyltin and triphenyltin are 104％, 99.3％ and 113％, and the detection limits are 0.33, 0.22 and 0.48 ng/g, respectively.The results are consistent with the certified value of CE 477 mussel tissue reference material.