电感耦合等离子体质谱法测定小麦籽粒中8种重金属元素

Determination of 8 Kinds of Heavy Metal Elements in Wheat Grains by Inductively Coupled Plasma Mass Spectrometry Method

以45Sc、72Ge、103Rh、115In、209Bi为内标元素,采用电感耦合等离子体质谱(ICP-MS)法同时测定农产品中铅(Pb)、镉(Cd)、铬(Cr)、铜(Cu)、砷(As)、汞(Hg)、镍(Ni)、锑(Sb) 8种重金属元素,选取2种国家标准物质菠菜(GBW10015)和柑橘叶(GBW10020)验证该方法的可靠性,并用该方法检测小麦籽粒中上述重金属含量,以期为农产品质量安全检测提供一种操作性强、高效、准确的方法。结果表明,该方法线性良好,相关系数均大于0.999 0,线性范围宽;铅、砷、铜、镍、铬检出限均为0.03 mg/kg,锑检出限为0.004 mg/kg,汞检出限为0.003 mg/kg,镉检出限为0.002 mg/kg。该方法加标回收率在63.7%～97.9%,精密度(RSD)在3.4%～15.1%。可靠性试验结果表明,该方法测定值均在标准值允许范围内。采用该方法检测小麦籽粒重金属含量表明,小麦中镍对高暴露人群可能存在较大的健康风险,其他元素安全风险级别较低。该方法简单、高效、准确,适用于农产品样品中8种重金属元素的快速检测。

The contents of lead(Pb),cadmium(Cd),chromium(Cr),copper(Cu),arsenic(As),mercury(Hg),nickel(Ni)and antimony(Sb)of agricultural products were determined with 45 Sc,72 Ge,103 Rh,115 In and 209 Bi as internal standard elements by microwave digestion-inductively coupled plasma mass spectrometry(ICP-MS)method.The national standard substances spinach(GBW10015)and citrus leaves(GBW10020)were selected to verify the reliability of this method,and the contents of the above heavy metals were determined in wheat grains,so as to provide an operational,efficient and accurate analytical measurement method for agricultural product quality and safety testing.The results showed that this method was well linear,the correlation coefficient was greater than 0.999 0,and the linear range was wide.The detection limits of lead,arsenic,copper,nickel,chromium were 0.03 mg/kg,which of antimony was 0.004 mg/kg,which of mercury was 0.003 mg/kg,which of cadmium was 0.002 mg/kg.The spiked recoveries of this method ranged from 63.7%to 97.9%,and the intra-laboratory precision(RSD)ranged from 3.4%to 15.1%.The reliability test results of the method showed that the measured values of this method were within the allowable range of the standard values.The results of contents of heavy metals in wheat grains measured by this method was as follows:nickel could have a large health risk to high-exposure populations,and other elements had lower safety risk.