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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-M P)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 m L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 m L乙二醇,减压浓缩并定容至1.0 m L,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2~3μg/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。
A solid-phase dispersion-high performance liquid chromatography (MSPD-HPLC) was developed for the determination of 2,4-DCP and 2-methyl- ) In three different types of soil residue analysis. Soil samples were added to the silica gel and homogenized, add 2.0 m L of distilled water inactivation, into the column, with dichloromethane elution. To the eluate was added 0.5 m L ethylene glycol, concentrated under reduced pressure and set to 1.0 m L, determined by HPLC. The results showed that the average recoveries of two analytes in the three soils ranged from 90% to 118% and the relative standard deviations (RSDs) ranged from 0.1% to 8.5% at 0.01-2.5 mg / kg The limit of detection (LOD) was between 2 ~ 3μg / kg, and the limit of quantification (LOQ) was 0.01 mg / kg. The recovery of 2,4-DCP and 4-C-2-MP by MSPD was higher than that of classical solid-liquid extraction (SLE). The recovery of two analytes in soil samples with different aging time was determined by MSPD-HPLC method, and the practicability of the method was verified. The method is simple, less solvent and analysis time is short, suitable for the determination of 2,4-DCP and 4-C-2-MP residues in soil.