乳业科学与技术 ›› 2024, Vol. 47 ›› Issue (1): 0-0.

• 分析检测 •    下一篇

ICP-MS法和GF-AAS法对乳粉中痕量铬检测测量系统的分析

冯灏   

  1. 湖北省食品质量安全监督检验研究院
  • 收稿日期:2024-04-09 修回日期:2024-04-29 出版日期:2024-01-01 发布日期:2024-05-21
  • 通讯作者: 冯灏

Analysis and research on the detection and measurement system of trace chromium in milk powder by ICP-MS method and GF-AAS method

  • Received:2024-04-09 Revised:2024-04-29 Published:2024-01-01 Online:2024-05-21

摘要: 目的:GB 5009.123-2023于2024-03-06实施,该标准中规定了食品中铬的两种常用检验方法:石墨炉原子吸收光谱法(GF-AAS)和电感耦合等离子体质谱法(ICP-MS)。GB 2762-2022中规定灭菌乳等液体乳、乳粉和调制乳粉中铬(以Cr计)限量。铬元素作为一种食品质量安全重点监测项目,提高乳制品中铬元素检测数据的准确性和可重复性,保障检测数据的可靠性,降低因检验过程造成的误判以及漏判风险是很有必要的。方法:本研究应用 Minitab 统计分析工具,运用控制图法、独立样件法、t检验法、方差分析法等研究方法,对这两种常用检验方法测量系统的稳定性、偏倚、线性、重复性与再现性进行研究分析。结果:两种检测方法测量系统极差图和均值图均无异常点,组内误差处于统计受控状态,稳定性良好;量具线性表和偏倚分析表结果均不存在显著的偏倚和显著的线性误差;量具(R&R)报告分析结果表明重复性和再现性良好;双因子方差分析表表明样品是唯一显著影响测量误差的因子;研究变异分析表表明测量系统误差可以接受。结论:ICP-MS法和GF-AAS法不仅能有效保障乳粉中铬元素含量检测数据的可靠性和可重复性,为实验室进行测量系统的误差分析与控制提供科学依据。同时也为乳制品中其他重金属检测以及其他食品中重金属检测的测量系统评价提供参考。

关键词: ICP-MS, GF-AAS, 乳粉, 铬, Minitab, 测量系统

Abstract: GB 5009.123-2023 "National Food Safety Standard Determination of Chromium in Foods" was implemented on 2024-03-06. The standard stipulates two commonly used testing methods for chromium in Purpose: GB 5009.123-2023 will be implemented on March 6, 2024. This standard specifies two commonly used testing methods for chromium in food: graphite furnace atomic absorption spectrometry (GF-AAS) and inductively coupled plasma mass spectrometry (ICP- MS).GB 2762-2022 stipulates the limit of chromium (calculated as Cr) in liquid milk such as sterilized milk, milk powder and prepared milk powder. As a key monitoring item for food quality and safety, chromium is very important to improve the accuracy and repeatability of chromium detection data in dairy products, ensure the reliability of detection data, and reduce the risk of misjudgment and missed determination caused by the inspection process necessary. Methods: This study applied Minitab statistical analysis tools and research methods such as control chart method, independent sample method, t test method, and variance analysis method to measure the stability, bias, linearity, and repeatability of the system using these two commonly used test methods. Conduct research and analysis on reproducibility. Results: There were no abnormal points in the range and mean charts of the measurement systems of the two detection methods. The errors within the group were under statistical control and the stability was good. There was no significant bias or significant difference in the results of the measuring instrument linear table and bias analysis table. linear error; the gage (R&R) report analysis results show that repeatability and reproducibility are good; the two-factor variance analysis table shows that the sample is the only factor that significantly affects the measurement error; the research variation analysis table shows that the measurement system error is acceptable. Conclusions: The ICP-MS method and GF-AAS method can not only effectively ensure the reliability and repeatability of chromium content detection data in milk powder, but also provide scientific basis for laboratory error analysis and control of measurement systems. It also provides a reference for the evaluation of measurement systems for the detection of other heavy metals in dairy products and the detection of heavy metals in other foods.

Key words: ICP-MS, GF-AAS, milk powder, chromium , Minitab, measurement system