原位自组装石墨烯固相微萃取探头的制备及其在水体苯系物分析中的应用

In-situ Preparation of a Solid Phase Microextraction Probe Based on Graphene Self-assembly and Its Application in Determination of Benzene Series in Water

利用石墨烯的自组装性能,原位制备了基于石墨烯材料的固相微萃取(SPME)探头,并结合气相色谱-质谱(GC-MS)建立了水体中甲苯、乙苯和邻二甲苯的分析方法。通过SEM对探头进行表征,发现制备的探头石墨烯材料均匀、牢固地结合在石英光纤上。通过优化萃取模式、萃取温度、萃取时间和盐度,得到最佳条件:顶空萃取模式、萃取温度为40℃、萃取时间为3 min、盐度为30%NaCl。在最佳条件下,3种苯系物在0.2~200μg/L范围内呈现出良好的线性,线性系数(r^2)为0.9987~0.9996;检出限为0.0012~0.0042μg/L;其相对标准偏差小于5%。对采集的3个样品进行测定,均不同浓度地测出了苯系物污染,其加标回收率为90.3%~111%。该方法可用于环境水样中挥发性苯系物的分析检测。

A solid-phase microextraction(SPME)probe based on graphene self-assembly was prepared in-situ,which was combined with GC-MS to develop a method for determination of toluene,ethylbenzene and o-xylene in water.SEM characterization results showed that graphene on the probe prepared was uniformly and firmly bonded to the quartz fiber.The effects of extraction mode,extraction temperature,extraction time and salinity were optimized.Under the optimum conditions,three benzenes showed good linearity in the concentration range of 0.2-200μg/L,with their linear coefficients(r^2)of 0.9987-0.9996.The limits of detection of this method ranged from 0.0012μg/L to 0.0042μg/L with relative standard deviations less than 5%.Three collected samples were detected to observe benzene series pollution with different concentrations.The spiked recoveries ranged from 90.3%to 111%.This method could be used for the determination of benzene series in environmental water samples.