气相色谱-质谱法同时测定烟用辅材中邻苯二甲酸酯与己二酸酯
Simultaneous GC-MS Determination of Phthalates and Adipates in Cigarette Auxiliary Materials
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摘要: 提出了用气相色谱-质谱法同时测定烟用辅材中7种邻苯二甲酸酯类和4种己二酸酯类增塑剂的含量。样品用异丙醇-环己烷(3+2)溶液超声提取,通过DB-5MS色谱柱分离,采用选择离子监测模式进行测定。11种增塑剂的质量浓度均在0.012~1.2 mg·L-1浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.022~0.038 μg·g-1之间。以不同种类的烟用辅材样品为基体,在3个浓度水平下进行回收试验,方法的回收率在84.0%~112%之间,测定值的相对标准偏差(n=5)在3.2%~8.5%之间。Abstract: A method for simultaneous determination of 11 plasticizers, including 7 phthalates and 4 adipates, in cigarette auxiliary materials by GC-MS was proposed. The sample was extracted ultrasonically with a mixture of isopropyl alcohol and cyclohexane (3+2). DB-5MS column was used for separation, and selected ion monitoring mode was adopted in MS measurement. Linear relationships between values of peak area and mass concentration of the 11 plasticizers were obtained in the same range of 0.012-1.2 mg·L-1, with limit of detection (3S/N) in the range of 0.022-0.038 μg·g-1. Tests for recovery and precision were made by standard addition method at 3 different concentration levels, values of recovery and RSD′s (n=5) found were in ranges of 84.0%-112% and 3.2%-8.5% respectively.