食用植物油中溶剂残留测定方法的优化

Optimization of determination method of solvent residue in edible vegetable oil

中文关键词:  溶剂残留  食用植物油  顶空-气相色谱

英文关键词:solvent residue  edible vegetable oil  headspace-gas chromatography

中文摘要:

      目的 优化食用植物油中溶剂残留的测定方法。方法 以“六号溶剂”溶液为标准品, 采用正庚烷纯品为内标, 样品经自动顶空进样器进行食用植物油样品前处理, 连接带氢火焰离子化检测器气相色谱仪对溶剂残留量进行测定。结果 改进后方法在10～200 mg/kg范围内线性关系良好, 相关系数为0.999; 方法的检出限为0.5 mg/kg, 定量限为1.6 mg/kg, 加标回收率为99.6%～102.3%,相对标准偏差为3.2%～4.6%。结论 该方法省去溶剂N,N-二甲基乙酰胺溶解内标正庚烷步骤, 改以正庚烷纯品为内标, 避免溶剂引入杂质同时极大缩短了样本检测周期, 适用于大批量食用植物油中溶剂残留的测定。

英文摘要:

      Objective To optimize the determination method of solvent residue in edible vegetable oil. Method Taking “solvent 6” solution as the standard, n-heptane purity as the internal standard, the sample was pre-treated by automatic headspace sampler for edible vegetable oil sample, and the residual solvent was determined by gas chromatograph with hydrogen flame ionization detector. Results The improved method had a good linear relationship in the range of 10 mg/kg to 200 mg/kg, and the correlation coefficient was 0.999. The limit of detection method was 0.5 mg/kg, the limit of quantification was 1.6 mg/kg, the recovery rates of spiked standard were 99.6%–102.3%, with the relative standard deviations of 3.2%–4.6%. Conclusion This method eliminates the step of dissolving the internal standard n-heptane with solvent N,N-dimethylacetamide, and uses pure n-heptane as the internal standard to avoid the introduction of impurities in the solvent and greatly shorten the sample detection cycle. It is suitable for determination of solvent residues in large bulk edible vegetable oils.