采用顶空固相微萃取-气相色谱-质谱法对饮用水源水中1,3,5-三氯苯进行了测定。以1,2-二氯苯-d4为内标,用PDMS萃取头顶空萃取20 min,萃取头于气相色谱进样口解析5 min。采用DB-624色谱柱在程序升温条件下进行分离,质谱分析中采用电子轰击离子源(230 ℃,70 eV)及选择离子监测模式测定。结果表明:1,3,5-三氯苯在0.100~2.50 μg·L-1范围内呈线性,检出限(3S/N)为0.019 μg·L-1。方法用于河流及水库水中的1,3,5-三氯苯的测定,加标回收率在91.5%~126.0%之间。

The content of 1,3,5-trichlorobenzene in drinking source water was determined by GC-MS with head-space solid phase micro-extraction (HS-SPME-GC/MS). Using 1,2-dichlorbenzene-d4 as internal standard, the 1,3,5-trichlorobenzene in water sample was extracted by SPME with the PDMS extractor for 20 min. The extractor was desorbed for 5 min at the inlet of the gas chromatograph, and separation of 1,3,5-trichlorobenzene was carried out on the DB-624 chromatographic column with programmed temperature elevation. Electron bombardment ionization (230 ℃, 70 eV) and selected ion scanning mode were adopted in MS analysis. Linearity was obtained in the range of 0.100-2.50 μg·L-1, with detection limit (3S/N) of 0.019 μg·L-1. The proposed method was applied to the determination of 1,3,5-trichlorobenzene in river water and reservoir water, and values of recovery obtained by standard addition method were in the range of 91.5%-126.0%.