气相色谱-质谱法测定木塞中10种多氯苯酚的残留量

Determination of 10 Polychlorinated Phenol Residues in Cork Stopper by GC-MS

采用气相色谱-质谱法同时测定木塞中10种多氯苯酚的残留量。样品经甲醇萃取后,在碳酸钾溶液中用乙酸酐乙酰化后再用正己烷萃取,萃取液经DB-5MS毛细管色谱柱分离,质谱分析中选择电子轰击正离子源和选择离子监测模式。10种多氯苯酚的线性范围为1.0~100.0mg·L^(-1),检出限(3S/N)在0.03~0.21mg·kg^(-1)之间.加标回收率在88.4%~104%之间,测定值的相对标准偏差(n=6)在2.1%~4.6%之间。方法用于市售木塞中10种多氯苯酚的测定,检出率为77.8%。

GC-MS was applied to the simultaneous determination of 10 polychlorinated phenol residues in Cork stoppers. Samples were extracted with methanol. After the extract was acetylated with acetic anhydride in a potassium carbonate solution, the mixture was extracted with n-hexane and separated on a DB-5MS capillary chromatographic column. El^＋ and SRM were adopted in MS analysis. The linearity range of 10 polychlorinated phenols was 1.0--100. 0 mg·L^-1, with detection limits （3S/N） in the range of 0. 03-0.21 mg · kg^-1. Recovery rates obtained by standard addition method were in the range of 88.4 %-104 %, and RSDs （n= 6） were in the range of 2.1%- 4. 6%. The method was used to determine 10 polychlorinated phenols in commercially available Cork stopper, giving the detection rate of 77.8%.