建立了简便、快速、有效的分散液-液微萃取-高效液相色谱-荧光检测(DLLME-HPLC-FLD)测定环境水样中15种多环芳烃(PAHs)的方法.重点探讨了萃取剂的种类和用量、分散剂的种类和用量以及萃取时间等对PAHs萃取效率的影响.在优化的条件下,评价了方法的可靠性.15种PAHs在0.01～10 μg/L 范围内呈良好的线性关系,相关系数r均不小于 0.991 3,峰面积的相对标准偏差(RSD)在2.3% ～4.7%之间(n=6).在优化条件下,富集因子和萃取回收率良好,分别为674～1 032 和67.4% ～103.2%,15种PAHs的检出限(S/N=3)在 0.000 3～0.002 μg/L 之间.建立的方法应用于敖江水样中PAHs的检测,平均加标回收率在79.5% ～92.3%之间,RSD在4.3% ～6.7%范围内(n=5).该方法适用于环境水样中痕量PAHs的分析.
A simple, rapid and effective method, the dispersive liquid-liquid microextraction coupled with high performance liquid chromatography-fluorescence detection (DLLME-HPLC-FLD), has been developed for the extraction and determination of polynuclear aromatic hydro-carbons (PAHs) in environmental water samples. The factors relevant to the microextraction efficiency, such as type and volume of dispersion agent and extraction solvents and the extrac-tion time were investigated and optimized. Under the optimized extraction conditions, the relia-bility of the proposed method was evaluated. The linear response of this method was in the range of 0. 01-10 μg/L (r≥0.991 3), the relative standard deviations (RSDs) of peak area for 0.05 μg/L PAHs were in the range of 2.3%-4. 7% (n = 6). At room temperature, the method exhibited excellent enrichment factors and good recoveries, 674-1 032 and 67. 4%-103. 2% respectively. The detection limits (S/N = 3) were in the range of 0. 000 3-0. 002 μg/L. The developed method was applied to the determination of 15 PAHs in the water from Aojiang river, the average recoveries were 79. 5%-92. 3% with RSD of 4. 3%-6. 7% (n=5). The developed method is suitable for the analysis of trace PAHs in environmental water samples.
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