气相色谱与质谱联用测定植物油溶剂残留的研究

Determination of Residual Oil Solvent Residue by Gas Chromatography and Mass Spectrometry

对比研究植物油中的六号溶剂残留量的填充柱气相色谱法、毛细管柱气相色谱法、气相色谱-质谱联用法三种分析方法。建立气相-质谱联用法,对该方法的国标适用性进行分析与验证,考察气质方法的线性范围、标准曲线相关系数、检出限、定量限、精密度、准确性、重复性及方法差异显著性等。确定了气质方法在0~200mg/kg浓度范围内线性关系良好。在10~160 mg/kg浓度范围的内加标回收试验中,回收率在98.2%~100.9%,相对标准偏差(n=6)小于3.0%。该方法的检出限为0.6 mg/kg,定量限为2.0 mg/kg。气质方法与毛细管气相色谱法测定结果无显著差异。

It was to compare three methods of packed column gas chromatography method,capillary column gas chromatography method and gas chromatography-mass spectrometry（GC-MS） method for the determination of No.6 solvent residues in vegetable oil.The method of GC-MS was established.The qualitative analysis and verification of the national standard of GC-MS method were carried out.The linear range,correlation coefficient,detection limit,limit of quantification,precision and accuracy of the method were investigated.The calibration curve was in the range of 0-200 mg/kg,and the linearity was good.The recoveries were 98.2%-100.9% in the range of 10-160 mg/kg,and the relative standard deviations（n=6） were less than 3.0%.The detection limit was 0.60 mg/kg,and the limit of quantitation was 2.0 mg/kg.