静态顶空-气相色谱-质谱法同时测定香精香料中14种有毒挥发性有机溶剂残留

Simultaneous Determination of 14 Toxic Volatile Organic Solvent Residues in Flavors and Fragrances by Static Headspace-Gas Chromatography-Mass Spectrometry

建立同时测定香精香料中14种常用挥发性有机溶剂残留(二氯甲烷、三氯甲烷、1,2-二氯乙烷、苯、四氯化碳、三氯乙烯、甲苯、四氯乙烯、氯苯、乙苯、间二甲苯、对二甲苯、邻二甲苯、异丙苯)的静态顶空-气相色谱-质谱分析方法。研究平衡温度和平衡时间等顶空条件,并对色谱参数和质谱条件进行优化。样品经80℃顶空温度提取30 min后,采用HP-1毛细管色谱柱(30 m×0.32 mm,0.25μm)分离,选择离子模式扫描测定。结果表明:14种挥发性有机物在0.5~50μg/L范围内线性关系良好,相关系数均大于0.998,平均加标回收率在71.7%~101.0%之间,相对标准偏差在1.71%~9.29%之间,方法检出限在1.0~10.0 ng/g之间。

A headspace-gas chromatography-mass spectrometry（SHS-GC-MS） method was presented for simultaneous determination of 14 toxic volatile organic solvent residues（dichloromethane,trichloromethane,1,2-dichloroethane,benzene,carbontetrachloride,trichloroethylene,methylbenzene,tetrachloroethylene,chlorobenzene,ethylbenzene,m-xylene,p-xylene,o-xylene,and isopropylbenzene） in flavors and fragrances.The headspace conditions including equilibrium temperature and time and the instrumental conditions were optimized.Samples were subjected to headspace extraction at 80 ℃ for 30 min and the extract was then separated on an HP-1 capillary column.and detected by GC-MS in the selected ion monitoring（SIM） mode.The results showed that in the range of 0.5–50 μg/L,all of the calibration curves displayed good linearity with correlation coefficients of higher than 0.998.The average recoveries of spiked samples were 71.7%–101.0% with relative standard deviation（RSD） between 1.71% and 9.29%.The limits of detection（LODs） were 1.0–10.0 ng/g.