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Talanta. 2014 Mar;120:289-96. doi: 10.1016/j.talanta.2013.12.005. Epub 2013 Dec 17.

Two-step microextraction combined with high performance liquid chromatographic analysis of pyrethroids in water and vegetable samples.

Author information

1
Materials Chemistry Research Unit, Department of Chemistry, Faculty of Science, Khon Kaen University, Khon Kaen 40002, Thailand.
2
Department of Physics, Faculty of Science, Khon Kaen University, Khon Kaen 40002, Thailand.
3
Materials Chemistry Research Unit, Department of Chemistry, Faculty of Science, Khon Kaen University, Khon Kaen 40002, Thailand. Electronic address: supalax@kku.ac.th.

Abstract

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.

KEYWORDS:

Dispersive liquid microextraction; Dispersive µ-solid phase extraction; High performance liquid chromatography; Magnetic nanoparticles; Pyrethroids

PMID:
24468372
DOI:
10.1016/j.talanta.2013.12.005
[Indexed for MEDLINE]

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