基于顶空-气相色谱-质谱法的食用油中润滑油挥发性组分快速筛查方法研究

Research on rapid screening method for volatile components of lubricating oil in edible oil based on headspace-gas chromatography-mass spectrometry

中文关键词:  顶空-气相色谱质谱法  食用油  润滑油  挥发性组分

英文关键词:headspace-gas chromatography-mass spectrometry  edible oil  lubricating oil  volatile components

中文摘要:

      目的 建立顶空-气相色谱-质谱法测定食用油中混入的润滑油挥发性组分的方法。方法 直接取1.0 g油样于10 mL顶空瓶中加盖密封, 在90 ℃平衡20 min的条件下顶空进样进行气相色谱-质谱仪检测, 以4-甲基-2-戊醇、异辛醇、壬烷、十一烷和十二烷5种化合物定性, 以异辛醇、壬烷、十一烷和十二烷4种化合物定量。结果 4种定量化合物在0.5~8.0 mg/kg范围内线性关系良好, 相关系数均大于0.9980。以大豆油为加标实验样品, 壬烷、异辛醇、十一烷和十二烷的加标回收率分别为91.5%~98.2%、81.9%~92.7%、92.8%~94.6%、89.3%~93.7%, 相对标准偏差均小于10%。在大豆油、花生油、菜籽油、玉米油、葵花籽油5种食用油中壬烷、异辛醇、十一烷和十二烷的检出限分别为0.006~0.013 mg/kg、0.016~0.045 mg/kg、0.011~0.020 mg/kg和0.020~0.036 mg/kg。结论 该方法具有操作简单、检测快速等优势, 对仪器要求不高, 一般实验室均能开展, 适用于食用油中微量润滑油污染的筛查。

英文摘要:

      Objective To establish a method for determining the volatile components of lubricating oil mixed in edible oil by headspace-gas chromatography-mass spectrometry. Methods The 1.0 g oil sample was directly taken into a 10 mL headspace bottle, then capped and sealed. Headspace-gas chromatography-mass spectrometry analysis was carried out at 90 ℃ equilibration for 20 min. Qualitative analysis was performed on 5 kinds of compounds: 4-methyl-2-pentanol, isooctanol, nonane, undecane and dodecane, while quantitative analysis was performed on isooctanol, nonane, undecane, and dodecane. Results The 4 kinds of quantitative compounds showed good linear relationships within the range of 0.5–8.0 mg/kg, and the correlation coefficients were all above 0.9980. Soybean oil was used as the sample for the spike recovery experiment. The recoveries of nonane, isooctanol, undecane, dodecane were 91.5%–98.2%, 81.9%–92.7%, 92.8%–94.6%, 89.3%–93.7% respectively and the relative standard deviations were all less than 10%. In the 5 kinds of edible oils: Soybean oil, peanut oil, rapeseed oil, corn oil and sunflower seed oil, the limits of detection of nonane, isooctanol, undecane, dodecane were 0.006–0.013 mg/kg, 0.016–0.045 mg/kg, 0.011–0.020 mg/kg, 0.020–0.036 mg/kg respectively. Conclusion This method has the advantages of simple operation and rapid detection, and does not have high requirements for the instrument, which can be carried out in general laboratories, and is suitable for the screening of trace lubricating oil contamination in edible oil.