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目的建立顶空固相微萃取-气相色谱-质谱法(HS-SPME-GC-MS)同时测定水中54种挥发性有机化合物的方法。方法采用HS-SPME-GC-MS法同时测定水中54种挥发性有机化合物,对影响固相微萃取效率的纤维涂覆种类、萃取温度、萃取时间、样品的离子强度、解吸温度和解吸时间进行了优化。结果用75μm CAR/PDMS(Carboxen/聚二甲基硅氧烷)作为萃取头,样品在(50±2)℃下萃取30 min,在气相色谱仪进样口温度为220℃下解吸3 min后进行GC-MS测定。方法的线性范围为1.0μg/L~100.0μg/L,相关系数为0.990~0.999,检测限为0.45μg/L~1.46μg/L。回收率为83.1%~117%,相对标准偏差为0.69%~17.6%。此法用于测定污水、自来水、净化水样品,检出7种卤代烷烃化合物,如三氯甲烷、二氯一溴甲烷、一氯二溴甲烷、三溴甲烷等。结论该法前处理步骤简单、快速、准确,可用于水中挥发性有机化合物测定。
Objective To establish a method for simultaneous determination of 54 volatile organic compounds in water by headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS). Methods Simultaneous determination of 54 volatile organic compounds in water by HS-SPME-GC-MS was performed on the types of fibers, the extraction temperature, the extraction time, the ionic strength, the desorption temperature and the desorption time Optimized. Results 75 μm CAR / PDMS (Carboxen / polydimethylsiloxane) was used as the extraction head. The sample was extracted at (50 ± 2) ℃ for 30 min and desorbed for 3 min at gas chromatograph inlet temperature of 220 ℃ GC-MS determination. The linear range of the method was 1.0μg / L ~ 100.0μg / L, the correlation coefficient was 0.990 ~ 0.999, and the detection limit was 0.45μg / L ~ 1.46μg / L. The recoveries were 83.1% ~ 117% with relative standard deviations of 0.69% ~ 17.6%. This method is used for the determination of sewage, tap water, purified water samples, detected 7 kinds of halogenated alkane compounds, such as chloroform, dichlorobromomethane, chlorinated dibromomethane, brominated methane and so on. Conclusion The pretreatment procedure of this method is simple, rapid and accurate and can be used for the determination of volatile organic compounds in water.