国家标准《食品中锡的测定》新增两方法的协同性试验研究

Collaborative Study on 2 Newly Added Methods in the National Standard of Determination of Tin in Foods

目的:组织8家实验室对《食品安全国家标准食品中锡的测定》(GB 5009.16—2023)新增的电感耦合等离子体质谱(Inductively Coupled Plasma Mass Spectrometry,ICP-MS)法和电感耦合等离子体发射光谱(Inductively Coupled Plasma Optical Emission Spectrometry,ICP-OES)法进行实验室间方法-性能协同性试验,为新标准方法的实施提供验证数据。方法:使用ICP-MS和ICP-OES对果汁等9种罐头食品进行锡元素含量测定。用Horwitz方程进行数据分析,对结果的相关参数和协同性试验指标进行评价。结果:两个方法的HorRat值均在2.0以下。其中,ICP-MS法的重复性相对标准偏差(RSDr)为2.26%~4.89%,再现性相对标准偏差(RSDR)为5.65%~11.70%;除了蔬菜泥的HorRat值为1.07,其余样本的HorRat值均在1.0以下;ICP-OES法的RSDr为1.71%~9.27%,RSDR为2.77%~13.10%,除了蔬菜泥的HorRat值为1.11,其余样本的HorRat值均在1.0以下。1个有证标准物质的测定结果在其标准值范围内,4个质控样测定结果均在其参考值范围内。结论:本次新增的ICP-MS和ICP-OES法,其实验室间协同性试验的精密度、准确度和稳定性均满足规定要求,适用于食品中锡含量的测定。

Objective:To validate characteristics of 2 newly added methods in the national standard of GB 5009.16—2023,eight laboratories were organized to participate in an inter-laboratory method-performance(collaborative)study on tin in foods by inductively coupled plasma mass spectrometry(ICP-MS)and inductively coupled plasma optical emission spectrometry(ICP-OES).Method:According to the methods of ICP-MS and ICP-OES provided by organizer,tin contents of 9 canned foods,namely,fruit juice,grapefruit,tomato paste,vegetable purees,lunch meat,canned marine fish,milk powder,flour and curry powder,were determined.The collaborative parameters on the measured results were analyzed and evaluated by Horwitz equation.Result:Both methods have HorRat values below 2.0.Repeatability relative standard deviation(RSDr)obtained by ICP-MS method ranged from 2.26%to 4.89%,while their reproducibility relative standard deviation(RSDR)ranged from 5.65%to 11.70%.The HorRat values of all samples were below 1.0 except vegetable puree(1.07).The RSDr byICP-OES method ranged from 1.71%to 9.27%,while RSDR ranged from 2.77%to 13.10%.The HorRat values were below1.0 except vegetable puree(1.11).The results of 1 certified reference material(CRM)were within the range of theircertificated value,and the results of 4 quality-controlled samples were within the range of their reference values.Conclusion:The newly added methods of ICP-MS and ICP-OES had satisfactory precision,accuracy and stability in theinter-laboratory collaborative study.They were suitable for the determination of tin in foods.