title: Application of QuEChERS method and gas chromatography-mass spectrometry for the analysis of cypermethrin residue in milk.
abstract: Analytical methods for the isolation and determination of cypermethrin in milk, based on the solid-phase microextraction (SPME) and QuEChERS methods (Quick, Easy, Cheap, Effective, Rugged, and Safe) are presented. The SPME technique was not appropriate to analyse cypermethrin in milk, even establishing the best extraction conditions, polydimethylsiloxane fiber, 60 min time extraction, 60 °C temperature extraction, addition of salt (NaCl) and stirring rate. The extraction efficiency was low probably because of the matrix constituents. The QuEChERS method involves the extraction of the analyte with acetonitrile and simultaneous liquid-liquid partitioning formed by adding anhydrous MgSO(4) plus NaCl, followed by the removal of residual water and cleanup using a procedure called dispersive solid-phase extraction, in which anhydrous MgSO(4) plus PSA and C18 are mixed with 1 mL of acetonitrile extract. The detection and quantification limits were 0.01 and 0.04 mg kg(-1), respectively, and the percentage recovery obtained ranged from 92 to 105% with relative standard deviations below 7%.
authors.affiliation: Embrapa Pecuária Sudeste, Rodovia Washington Luiz, São Carlos-SP, Brazil. shgb@uol.com.br
authors.forename: Silvia H G
authors.initials: SH
authors.lastname: Brondi
authors.forename: Adriana N
authors.initials: AN
authors.lastname: De Macedo
authors.forename: Gilberto B
authors.initials: GB
authors.lastname: de Souza
authors.forename: Ana R A
authors.initials: AR
authors.lastname: Nogueira
mesh_terms: D000818:Animals; D002417:Cattle; D005591:Chemical Fractionation / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D008892:Milk / Q000737:chemistry*; D010573:Pesticide Residues / Q000032:analysis*; D011722:Pyrethrins / Q000032:analysis*
chemical_list: D010573:Pesticide Residues; D011722:Pyrethrins; C017160:cypermethrin