提出了气相色谱-质谱法测定塑料玩具中16种多环芳烃(PAH′s)含量的方法。样品经正己烷超声提取30 min后,40 ℃水浴氮气吹干。用水、甲醇和正己烷-二氯甲烷(3+2)混合溶剂各5 mL溶解残渣,过C18固相萃取柱净化,用正己烷-二氯甲烷(3+2)混合溶液洗脱,所得洗脱液过HP-5MS色谱柱分离,电子轰击离子源检测。16种多环芳烃的质量浓度在0.2~4.0 mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.002~0.021 mg·kg-1之间。以聚丙乙烯、聚乙烯、聚氯乙烯或丙烯腈-丁二烯-苯乙烯共聚物等4种材质的塑料玩具为基体,进行加标回收试验,回收率在79.6%~95.2%之间。

GC-MS was applied to the determination of 16 polycyclic aromatic hydrocarbons (PAH′s) in plastic toys. Sample was extracted ultrasonically with n-hexane for 30 min, and the extract was evaporated to dryness in a water bath at 40 ℃ by N2-blowing. The residue was dissolved with 5 mL of H2O, 5 mL of CH3OH and 5 mL of mixture of n-hexane and CH2Cl2(3+2), and purified by passing through C18 SPE column and eluted with mixed solvent of n-hexane-CH2Cl2(3+2). The analyte were separated on HP-5MS column and EI source was used in MS. Linear relationships between values of peak area and mass concentration of the 16 PAH′s were kept in the same range of 0.2-4.0 mg·L-1, with detection limits (3S/N) in the range of 0.002-0.021 mg·kg-1. Tests for recovery were made by standard addition method with 4 kinds of plastic toys (made with PP, PE, PVC or ABS) as matrixes, values of recovery found were in the range of 79.6%-95.2%.