菜籽油中溶剂残留量测定方法验证及不确定度评定
Method Validation and Uncertainty Evaluation for the Determination of Solvent Residues in Rapeseed Oil
摘要
植物油中溶剂残留量是评价油脂质量好坏的一项重要指标,国家标准采用顶空-气相色谱法测定,依据 GB/T 27404-2008《实验室质量控制规范 食品理化检测》、GB/T 32465-2015《化学分析方法验证确认和内部质量控制要求》对菜籽油中溶剂残留量进行方法学验证;依据 JJF 1059.1-2012《测量不确定度评定与表示》对菜籽油中溶剂残留量的测量不确定度进行评定,为检测结果可靠性提供支撑.结果表明:溶剂残留量线性范围、检出限和定量限、加标回收率和精密度等实验结果均满足国标要求,本实验室具备准确执行 GB 5009.262-2016《食品安全国家标准食品中溶剂残留量的测定》测定植物油中溶剂残留量的能力;菜籽油中溶剂残留量为10.6 mg/kg 时,其扩展不确定度为 2.8 mg/kg(k=2).标准曲线变动性、标准系列溶液配制、标准物质引入的不确定度较大,需要在今后实验中优化改进,进一步减小不确定度,保证检验工作质量.
Solvent residue is an important indicator of vegetable-oil quality and is determined by headspace gas chromatography in the relevant national standard.In accordance with GB/T 27404-2008,Criteria on Quality Con-trol of Laboratories—Chemical Testing of Food,and GB/T 32465-2015,Requirements for Verification and Valida-tion of Chemical Analysis Methods and for Internal Quality Control,the method for determining solvent residues in rapeseed oil was validated.Measurement uncertainty was evaluated in accordance with JJF 1059.1-2012,Evalua-tion and Expression of Uncertainty in Measurement,to support the reliability of the test results.The linear range,limit of detection,limit of quantification,spiked recovery,and precision met the requirements of the national standard,demonstrating that the laboratory was capable of accurately applying GB 5009.262-2016,National Food Safety Standard—Determination of Solvent Residues in Foods,to determine solvent residues in vegetable oils.When the solvent residue in rapeseed oil was 10.6 mg/kg,the expanded uncertainty was 2.8 mg/kg(k=2).Variability in the calibration curve,preparation of the calibration solutions,and uncertainty introduced by the refer-ence material were the major uncertainty sources and should be further controlled to reduce measurement uncertain-ty and ensure the quality of testing.
年，卷(期)：
2026, 55(4)
分类号：
TS225.1
机标分类号：
TS207.53
R927
O657.71
在线出版日期：
2026年9月15日
