磁分散固相微萃取气相色谱法测定苯系物研究

Magnetic Dispersed Solid Phase Microextraction Couple with Gas Chromatography for Determining Trace Benzene,Toluene,Ethylbenzene and Xylenes in Water Samples

本研究通过溶胶凝胶法制备了新型四氧化三铁@二氧化硅@氧化石墨烯(Fe_3O_4@SiO_2@GO)核壳结构的磁分散固相微萃取(MDSPME)吸附剂,并将其应用于水样中痕量苯系物的测定.通过实验对吸附剂用量、吸附时间、转速、解析剂种类和体积、脱附时间等参数进行优化.筛选出最佳萃取条件为:称取60 mg吸附剂于进样瓶中,加入20mL五苯(苯、甲苯、乙苯、二甲苯、苯乙烯)混标溶液,在200 r/min的转速下吸附1 min,然后加入1 mL丙酮解析1min,最后移取1.00μL待测液进行分析.在优化萃取条件下,得出本实验具有1.0-40.0μg/mL的线性范围,R^2≥0.9873,检出限为0.3-0.5μg/L,应用于水样检测中的加标回收率为81.6%-108.9%.综上所述,该方法具有萃取时间短、效率高,所需药品用量少和灵敏度高等优点.

A novel Fe3O4@SiO2@GO magnetic dispersed solid phase microextraction（MDSPME） adsorbent was prepared by sol-gel method, Adsorbent was applied to the determination of benzene, toluene, ethylbenzene and xylenes, styrene（BTEXS）in water samples. The effects of the parameters such as the amount of adsorbent, extraction time, speed, type of reagent and volume, the time of desorption on extraction efficiency were investigated experimentally. Experiments showed that the optimized extracting condition were 60 mg of adsorbent, revolution of 200 r/min, adsorption of 1 min, acetone as a desorbent solvent, desorbent in an amount of 1 mL. At last, the solution was analyzed by the gas chromatography with the solution of 1μl. Under the optimized conditions, linear relationship between values area and mass concentration of the seven benzene homologues were kept in the range of 1-40 μg/mL, with detection limits of 0.3-0.5 μg/L, The proposed method was applied to the analysis of 3 environmental water samples, giving values of recovery found by standard by standard addition method in the range of 81.6-108.9%. In a word, it is a convenient and efficient method for the detection of the water samples with little sample volume, high concentration efficiency and high sensitivity.