A novel method for the determination of sixteen polycyclic aromatic hydrocarbons (PAHs) in environmental water samples was developed using column clean-up (CCU) coupled with continuous flow single drop microextraction (CF-SDME) prior to the determination by gas chromatography-mass spectrometry (GC–MS). In this method, purification, extraction and enrichment were carried out in a single step, which reduced the effect of most organic interferents on the determination of target analytes, greatly simplified the operation process and shortened the whole pre-treatment time. The CCU-CF-SDME system was first used, and shortcomings such as long extraction time, instability of suspended microdrop of the traditional SDME system were overcome. The influences of several experimental parameters, including the type and amount of column packing material, the type and volume of extraction solvent, the flow rate of sample solution, extraction temperature, pH and ionic strength of sample solution, on the extraction efficiency were investigated. Under the optimal experimental conditions, the good linearities were obtained in the concentration range of 0.02–10 μg L⁻¹ with correlation coefficients ranging from 0.9912 to 0.9995 for all the analytes. The limits of detection and quantification of the analytes were in the range of 0.0012–0.0101 μg L⁻¹ and 0.0041–0.0336 μg L⁻¹, respectively. The pre-concentration factors in the range of 777–978 for the PAHs were obtained. The proposed method was applied on the analysis of environmental water samples, and the recoveries of target analytes were in the range of 81.8–105.8% with the relative standard deviations ranging from 0.5% to 6.4%. The results showed that the developed method was a simple, quick and feasible method for the determination of PAHs in environmental water samples.

建立了一种在气相色谱-质谱法测定之前使用柱净化（CCU）和连续流单滴微萃取（CF-SDME）联用测定环境水样品中十六种多环芳烃（PAHs）的新方法。 （GC–MS）。该方法只需一步即可进行纯化，提取和富集，从而减少了大多数有机干扰物对目标分析物测定的影响，大大简化了操作过程并缩短了整个预处理时间。首次使用CCU-CF-SDME系统，克服了传统SDME系统提取时间长，悬浮微滴不稳定等缺点。几个实验参数的影响，包括柱填充材料的类型和数量，研究了萃取溶剂的种类和体积，样品溶液的流量，萃取温度，pH和样品溶液的离子强度对萃取效率的影响。在最佳实验条件下，在0.02–10μgL的浓度范围内可获得良好的线性^-1，所有分析物的相关系数在0.9912至0.9995的范围内。分析物的检出限和定量限分别为0.0012–0.0101μgL ^-1和0.0041–0.0336μgL ^-1。获得了多环芳烃的预浓缩因子，范围为777–978。该方法用于环境水样的分析，目标分析物的回收率在81.8％至105.8％之间，相对标准偏差在0.5％至6.4％之间。结果表明，所建立的方法是测定环境水样中多环芳烃的一种简便，快捷，可行的方法。