Determination of 2,4-dichlorophenol and 4-chloro-2-methylphenol residues in soil by matrix solid-phase dispersion and high performance liquid chromatography
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摘要: 建立了基质固相分散-高效液相色谱法(MSPD-HPLC)测定2,4-二氯苯酚(2,4-DCP)和2-甲基-4-氯苯酚(4-C-2-MP)在3种不同类型土壤中残留量的分析方法。土壤样品加入硅胶研匀后,加入2.0 mL蒸馏水使其失活,装入层析柱,用二氯甲烷洗脱。向洗脱液中加入0.5 mL乙二醇,减压浓缩并定容至1.0 mL,HPLC测定。结果表明:在0.01～2.5 mg/kg添加水平下,3种土壤中两种待测物的平均回收率在90%～118%之间,相对标准偏差(RSD)在0.1%～8.5%之间;检测限(LOD)在2～3 μg/kg之间,定量限(LOQ)均为0.01 mg/kg。与经典的固-液萃取法(SLE)相比,MSPD法对2,4-DCP和4-C-2-MP的提取回收率较高。通过MSPD-HPLC法测定不同老化时间土壤样品中两待测物的回收率,验证了该方法的实用性。该法操作简单、溶剂用量少、分析时间短,适合用于土壤中2,4-DCP和4-C-2-MP残留量的检测。Abstract: Matrix solid-phase dispersion and high performance liquid chromatography(MSPD-HPLC)was ultilized to determine 2,4-dichlorophenol(2,4-DCP) and 4-chloro-2-methylphenol(4-C-2-MP) residues in three different types of soil. Soil sample and silica gel were manually blended together, followed by addition of 2.0 mL distilled water. Samples were introduced into glass column, and eluted with dichloromethane. Then 0.5 mL ethylene glycol was added into the extract. The solution was concentrated and diluted to 1.0 mL. Samples were analyzed by HPLC-DAD. The recoveries of two analytes in three different soils ranged from 90% to 118%, with relative standard deviation(RSD) from 0.1% to 8.5% at spiked level ranged from 0.01 to 2.5 mg/kg. Limits of quantifications(LOQs) of this method were 0.01 mg/kg. Limits of detections(LODs) reached 2-3 μg/kg. The recovery tests of MSPD method and classical SLE method showed that with MSPD high recovery could be achieved. This MSPD-HPLC-DAD method was also applied to analytes recoveries of soils at different aging times. In conslusion, this method is characterized by simple, analysis time saving, less solvent consumption and is suitable for residues analysis of 2,4-DCP and 4-C-2-MP in soils.
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