电感耦合等离子体质谱法同时测定海产品中19种矿物元素

Simultaneous Determination of 19 Mineral Elements in Seafood by Inductively Coupled Plasma Mass Spectrometry

建立电感耦合等离子体质谱(inductively coupled plasma mass spectrometry,ICP-MS)同时测定海产品中镁、钾、钒、铬、锰、铁、镍、铜、锌、锗、砷、硒、镉、锡、锑、铽、汞、铅和铋共19种矿物元素的分析方法。样品在硝酸-过氧化氢体系中经微波消解后直接上样分析,采用八极杆碰撞-反应池技术(octopole collisionreaction system,ORS)消除了多原子离子质谱干扰,以钪、铑、铟、铱作为内标元素校正了质谱分析中基体效应并补偿了信号漂移。结果表明:测定质量浓度在0~50 mg/L范围内,各元素呈现良好的线性关系,相关系数均在0.999 5以上;检出限为0.004~80.110?μg/L。选择国家一级标准物质扇贝(GBW10024)、大虾(GBW10050)和牡蛎(GBW10068)验证方法的可靠性,待测元素测定结果均在标准值允许范围内,日间相对标准偏差在0.8%~15.2%之间。

An analytical method based on inductively coupled plasma mass spectrometry（ICP-MS） has been developed for the simultaneous determination of 19 mineral elements（Mg, K, V, Cr, Mn, Fe, Ni, Cu, Zn, Ge, As, Se, Cd, Sn, Sb, Tb, Hg, Pb and Bi） in seafood. After the samples were pretreated by microwave digestion with HNO3-H2O2, octopole collisionreaction system（ORS） was used to eliminate the polyatomic interferences. Sc, Rh, In and Ir were used as internal standard elements to compensate matrix effect and signal drift. The results indicated that the concentrations and responses of each element showed a good linear relationship in the range of 0–50 mg/L with correlation coefficient no less than 0.9995. The limits of detection（LOD） were in the range of 0.004–80.110 μg/L. The established method was validated by using it to analyze the national standard reference materials of scallop（GBW10024）, prawn（GBW10050） and oyster（GBW10068） and it turned out that the relative standard deviation values of reproducibility（n = 6） were 0.8%–15.2%,and the analysis results were all in the reference ranges.