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
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摘要: 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0.02~10.0 mg·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。Abstract: 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 0.02-10.0 mg·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.