[目的]采用固相萃取-高效液相色谱法测定废水中4种氯苯类有机污染物.[方法]利用固相萃取技术,结合高效液相色谱法(PDA检测器)分析废水中4种氯苯类有机污染物,比较了ODS-C18、Sep-Park Vac Silica、Bond Elut CARBON、Bond Elut SI和Bond Elut PLEXA 5种SPE小柱对4种氯苯类的萃取效率,并系统研究了最佳萃取条件.[结果]氯苯、1,4-二氯苯和1,2,4-三氯苯的紫外检测波长为210 nm,而1,2-二氯苯的检测波长为224 nm;通过比较5种SPE小柱的萃取效率,发现ODS-C18小柱有很好的回收率.甲醇的最佳洗脱体积为4.0 ml;除氯苯外,其他氯苯类化合物的穿透体积都在1.0L以上,而氯苯的穿透体积为250 ml,表明ODS-C18小柱对二氯苯和三氯苯具有很强的吸附性.在最佳萃取和测定条件下,该方法线性范围为0.005 ～0.100 mg/L,检出限为0.076～0.105 μg/L,完全满足日常环境监测分析要求.[结论]该研究为氯苯类环境监测分析提供了参考.%[Objective] The study aims to determine four chlorobenzene compounds in waste water by SPE-HPLC.[Method] A method for determination of four chlorobenzene compounds in waste water by solid phase extraction with HPLC-PAD detection was investigated,then the extraction efficiency of four chlorobenzene compounds by five SPE columns (ODS-C18,Sep-Park Vac Silica,Bond Elut CARBON,Bond Elut SI and Bond Elut PLEXA) was compared,finally the optimal extraction conditions were discussed.[Result] The UV detection wavelength of chlorobenzene,1,4-DCB and 1,2,4-TCB was 210 nm,but that of 1,2-DCB was 224 nm.Among the five SPE columns,ODS-C18 column has the best recovery.4.0 ml methanol is as eluting solvent; the breakthrough volume of most compounds is above 1.0 L,but that of chlorobenzene is 250 ml,showing that ODS-C18 column has a strong adsorption to dichlorobenzene and trichlorobenzene.Under the optimized conditions,the linear range was 0.005-0.100 mg/L,and the detection limit was 0.076-0.105 μg/L,which fully meets the requirements of daily environmental monitoring and analysis.[Conclusion] The research can provide references for monitoring and analysis of chlorobenzene compounds.
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