提出了固相微萃取-气相色谱-质谱法测定水体中24种半挥发性有机污染物(SVOC′s)含量的方法。为使固相微萃取达到更高的效率,选用85 μm聚丙烯酸酯纤维作为微萃取头的涂层,萃取温度及时间分别为50 ℃和30 min。用DB-5MS毛细管色谱柱分离,电子轰击离子源全扫描监测模式检测。24种SVOC′s的质量浓度在1.0~40 μg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.11~0.39 μg·L-1之间。采用标准加入法进行回收试验,方法的回收率在51.0~95.8%之间,相对标准偏差(n=7)均小于16%。

GC-MS with solid phase micro-extraction (SPME) was applied to the determination of 24 semi-volatile organic contaminants (SVOC′s) in water. To attain a higher efficiency in SPME, 85 μm polyacrylate fibre was selected as coating for the micro-extractor, and the extraction was carried out at 50 ℃ for 30 min. The analyte were separated on DB-5MS capillary column and detected by EI ion source with whole scanning monitoring mode. Linear relationships between values of peak area and mass concentration of the 24 SVOC′s were kept in the same range of 1.0-40 μg·L-1. Detection limits (3S/N) found were ranged from 0.11 to 0.39 μg·L-1. Tests for recovery were performed by addition of mixed standards of the 24 SVOC′s for 7 parallel determinations each, results of average recovery found were in the range of 51.0%-95.8% with RSD′s (n=7) less than 16%.