Materials Chemistry Research Unit, Department of Chemistry, Faculty of Science, Khon Kaen University, Khon Kaen 40002, Thailand.
Department of Physics, Faculty of Science, Khon Kaen University, Khon Kaen 40002, Thailand.
Talanta. 2014 Mar;120:289-96. doi: 10.1016/j.talanta.2013.12.005. Epub 2013 Dec 17.
Dispersive liquid microextraction (DLME) combined with dispersive µ-solid phase extraction (D-µ-SPE) has been developed as a new approach for the extraction of four pyrethroids (tetramethrin, fenpropathrin, deltamethrin and permethrin) prior to the analysis by high performance liquid chromatography (HPLC) with UV detection. 1-Octanol was used as the extraction solvent in DLME. Magnetic nanoparticles (Fe3O4) functionalized with 3-aminopropyl triethoxysilane (APTS) were used as the dispersive in DLME and as the adsorbent in D-µ-SPE. The extracted pyrethroids were separated within 30 min using isocratic elution with acetonitrile:water (72:28). The factors affecting the extraction efficiency were investigated. Under the optimum conditions, the enrichment factors were in the range of 51-108. Linearity was obtained in the range 0.5-400 ng mL(-1) (tetramethrin) and 5-400 ng mL(-1) (fenpropathrin, deltamethrin and permethrin) with the correlation coefficients (R(2)) greater than 0.995. Detection limits were 0.05-2 ng mL(-1) (water samples) and 0.02-2.0 ng g(-1) (vegetable samples). The relative standard deviations of peak area varied from 1.8 to 2.5% (n=10). The extraction recoveries of the four pyrethroids in field water and vegetable samples were 91.7-104.5%. The proposed method has high potential for use as a sensitive method for determination of pyrethroid residues in water and vegetable samples.
分散液液微萃取（DLME）结合分散微固相萃取（D-µ-SPE）已被开发为一种新方法，用于在高效液相色谱（HPLC）与紫外检测分析之前萃取四种拟除虫菊酯（四甲菊酯、氯菊酯、溴氰菊酯和氯菊酯）。1-辛醇被用作 DLME 的萃取溶剂。用 3-氨丙基三乙氧基硅烷（APTS）功能化的磁性纳米粒子（Fe3O4）被用作 DLME 的分散剂和 D-µ-SPE 的吸附剂。采用乙腈：水（72:28）等度洗脱，在 30 分钟内分离提取的拟除虫菊酯。研究了影响萃取效率的因素。在最佳条件下，富集因子在 51-108 范围内。在 0.5-400ng mL(-1)（四甲菊酯）和 5-400ng mL(-1)（氯菊酯、溴氰菊酯和氯菊酯）范围内得到了线性关系，相关系数（R(2)）大于 0.995。检测限为 0.05-2ng mL(-1)（水样）和 0.02-2.0ng g(-1)（蔬菜样品）。峰面积的相对标准偏差在 1.8-2.5%（n=10）之间变化。四种拟除虫菊酯在田间水和蔬菜样品中的萃取回收率为 91.7-104.5%。该方法具有用于测定水样和蔬菜样品中拟除虫菊酯残留的高灵敏度方法的潜力。
