微波消解-ICP-MS法测定水产罐头食品中12种元素

Determination of 12 Elements in Aquatic Canned Food by Inductively Coupled Plasma Mass Spectrometry with Microwave Digestion

试验旨在建立微波消解-电感耦合等离子体质谱(ICP-MS)同时测定水产罐头食品中铅、砷、镉、铬、汞、钒、镍、锰、铜、锡、铁、铝共12种元素的分析方法。样品以硝酸-过氧化氢作为消解体系,经微波消解处理后用ICP-MS检测,以钪(45Sc)、锗(74Ge)、铟(115In)、铋(209Bi)作为内标元素校正基体效应,采用标准曲线法定量。结果表明, 12种元素的线性相关系数均大于0.999,检出限为0.000 63~0.065 mg/kg,定量限为0.002 1~0.22 mg/kg。各元素加标浓度在0.01~8 mg/kg范围内,加标回收率在89.6%~101.6%之间,相对标准偏差(RSD)为1.03%~5.36%(n=6)。国家标准物质中各元素的测定值与标准值均相吻合。该方法操作简单,分析速度快,测量灵敏度高,结果准确、可靠,适用于大批量水产罐头食品中多元素的同时测定。

It was to establish a method for the simultaneous determination of 12 elements(Pb, As, Cd, Cr, Hg, V, Ni, Mn, Cu, Sn, Fe and Al) in aquatic canned food by inductively coupled plasma mass spectrometry with microwave digestion. The samples were digested by microwave digestion using hydrogen-peroxide as a digestion system, followed by the ICP-MS analysis. 45Sc, 74Ge, 115In and 209Bi were used as internal standard elements to compensate matrix effect. The concentrations of samples were calculated according to the standard curve. The linear correlation coefficients for all elements were more than 0.999. The detection limits were 0.000 63-0.065 mg/kg and the quantification limits were 0.002 1-0.22 mg/kg. The recoveries of spiked samples were in the range of 89.6%-101.6% and the relative standard deviations(RSDs) were 1.03%-5.36%(n=6) at spiked levels of 0.01-8 mg/kg. The measured values of the national standard materials were in agreement with the certified values. This method was simple, quick, sensitive and accurate. It was suitable for the simultaneous analysis of various elements in large quantities of aquatic canned food.