虾蛄中15种元素的微波消解-电感耦合等离子体质谱测定法

Determination of 15 elements in Oratosquilla oratoria by microwave digestion and inductively coupled plasma-mass spectrometry

目的建立虾蛄中锂、铝、钒、铬、锰、镍、铜、砷、硒、镉、锡、锑、钡、汞和铅的微波消解-电感耦合等离子体质谱测定方法。方法通过比较湿法消解和微波消解,选定微波消解处理虾蛄样品,电感耦合等离子体质谱法(ICP-MS)测定,碰撞反应池技术消除干扰,内标法定量。结果相关系数均≥0.9993,检出限为0.0005~0.0100 mg/kg,回收率为82%~115%,RSD为0.8%~4.5%,标准物质中各元素检测结果符合要求。14份虾蛄中镉均标超;砷为2.81~4.94 mg/kg,高于一般食品;铜、铬、汞和铅含量低于限量值;锂、铝、钒、锰、镍、硒、锡、锑、钡分别为0.072~0.140、0.43~7.36、0.0078~0.0240、0.51~2.28、0.0075~0.1400、0.50~1.17、0.011~0.033、0.0010~0.0041和0.11~0.34 mg/kg。结论该方法分析速度快,干扰小,准确度高,精密度好,适用于虾蛄中多种元素的快速测定和定量分析。

Objective To establish a method for simultaneous determination of 15 elements,including lithium,aluminum,vanadium,chromium,manganese,nickel,copper,arsenic,selenium,cadmium,tin,antimony,barium,mercury,and lead,in Oratosquilla oratoria by microwave digestion and inductively coupled plasma-mass spectrometry.Methods By comparing wet digestion and microwave digestion,microwave digestion was selected to digest the samples of Oratosquilla oratoria,and the elements were determined by inductively coupled plasmamass spectrometry(ICP-MS).Collision reaction cell technology was used to eliminate interference and the quantification was based on the internal standard curves.Results The correlation coefficients were above 0.9993.The limit of detection was 0.0005-0.0100 mg/kg,and the recovery rates were 82%-115%,with RSD between0.8%and 4.5%.The determination values of the national standard reference materials met the requirements.The contents of cadmium in 14 Oratosquilla oratoria samples exceeded the limit.The arsenic content was 2.81-4.94 mg/kg,which was than that of general food.The contents of copper,chromium,mercury and lead were below the limit values.The contents of lithium,aluminum,vanadium,manganese,nickel,selenium,tin,antimony and barium were 0.072-0.140,0.43-7.36,0.0078-0.0240,0.51-2.28,0.0075-0.1400,0.50-1.17,0.011-0.033,0.0010-0.0041 and 0.11-0.34 mg/kg,respectively.Conclusion This method has the advantages of high analytical speed,less interference,good accuracy and high precision,and it is suitable for the rapid determination and quantitative analysis of various elements in Oratosquilla oratoria.