层析净化-气相色谱-质谱法测定烟叶中6种邻苯二甲酸酯

GC-MS Determination of 6 Phthalates in Tobacco Leaves with Chromatographic Purification

采用层析净化-气相色谱-质谱法测定烟叶中6种邻苯二甲酸酯的含量。烟叶样品经正己烷-丙酮(1+1)溶液超声提取,过硅胶层析柱,以正己烷-丙酮(9+1)混合液洗脱净化,在气相色谱分离中用DB-5MS毛细管柱为固定相,在质谱分析中采用选择离子监测模式。6种邻苯二甲酸酯的质量浓度均在0.02~10.0mg·L^(-1)范围内与其峰面积呈线性关系。方法用于烟叶样品分析,加标回收率在81.6%~107%之间,测定值的相对标准偏差(n=6)在3.2%~9.8%之间。

GC-MS with chromatographic purification was applied to the determination of 6 phthalates in tobacco leaves.The sample of tobacco leaves was extracted ultrasonically with n-hexane-acetone（1＋1）mixture,and purified on silica-gel column with a mixture of n-hexane-acetone（9＋1）as eluant.DB-5MS capillary column was used for GC separation and the selected ion monitoring mode was adopted in MS determination.Linear relationships between values of peak area and mass concentration of the 6 phthalates were kept in the same range of 0.02-10.0mg·L^-1.The proposed method was applied to the analysis of samples of tobacco leaves,giving values of recovery and RSD′s（n=6）in the ranges of 81.6%-107% and 3.2%-9.8% respectively.