Determination of neonicotinoid insecticides in environmental samples by micellar electrokinetic chromatography using solid-phase treatments

被引:26
|
作者
Ettiene, Gretty [2 ]
Bauza, Roberto [3 ]
Plata, Maria R. [1 ,4 ]
Contento, Ana M. [1 ]
Rios, Angel [1 ,4 ]
机构
[1] Univ Castilla La Mancha, Dept Analyt Chem & Food Technol, E-13071 Ciudad Real, Spain
[2] Univ Zulia, Fac Agron, Dept Chem, Maracaibo 4011, Venezuela
[3] Univ Zulia, Fac Sci, Dept Chem, Maracaibo 4011, Venezuela
[4] IRICA Reg Inst Appl Sci Res, Ciudad Real, Spain
关键词
Environmental samples; Matrix solid-phase dispersion; Micellar electrokinetic chromatography; Neonicotinoids; Solid-phase extraction; LIQUID-CHROMATOGRAPHY; PESTICIDE-RESIDUES; 6-CHLORONICOTINIC ACID; EXTRACTION CLEANUP; MASS SPECTROMETRY; SOIL SAMPLES; DISPERSION; WATER; VEGETABLES; GREENHOUSE;
D O I
10.1002/elps.201200241
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A sensitive and reliable method based on MEKC has been developed and validated for trace determination of neonicotinoid insecticides (thiamethoxam, acetamiprid, and imidacloprid) and the metabolite 6-chloronicotinic acid in water and soil matrices. Optimum separation of the neonicotinoid insecticides was obtained on a 58 cm long capillary (75 mu m id) using as the running electrolyte 40 mM SDS, 5 mM borate (pH 10.4), and 5% (v/v) methanol at a temperature of 25 degrees C, a voltage of 25 kV and with hydrodynamic injection (10 s). The analysis time was less than 7 min. Prior to MEKC determination, the samples were purified and enriched by carrying out extraction-preconcentration steps. For aqueous samples, off-line SPE with a sorptive material such as Strata-X (polymeric hydrophobic sorbent) and octadecylsilane (C18) was carried out to clean up and preconcentrate the insecticides. However, for soil samples, matrix solid-phase dispersion (MSPD) was applied with C18 used as the dispersant. Good linearity, accuracy, and precision were obtained and the detection limits were in the range between 0.01 and 0.07 mu g mL-1 for river water and 0.17 and 0.37 mu g g-1 for soil samples. Recovery levels reached greater than 92% for all of the assayed neonicotinoids in river water samples with Strata-X. In soil matrices, the best recoveries (6399%) were obtained with MSPD.
引用
收藏
页码:2969 / 2977
页数:9
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