title: Single solid phase extraction method for the simultaneous analysis of polar and non-polar pesticides in urine samples by gas chromatography and ultra high pressure liquid chromatography coupled to tandem mass spectrometry.
abstract: A new multiresidue method has been developed and validated for the simultaneous extraction of more than two hundred pesticides, including non-polar and polar pesticides (carbamates, organochlorine, organophosphorous, pyrethroids, herbicides and insecticides) in urine at trace levels by gas and ultra high pressure liquid chromatography coupled to ion trap and triple quadrupole mass spectrometry, respectively (GC-IT-MS/MS, UHPLC-QqQ-MS/MS). Non-polar and polar pesticides were simultaneously extracted from urine samples by a simple and fast solid phase extraction (SPE) procedure using C(18) cartridges as sorbent, and dichloromethane as elution solvent. Recovery was in the range of 60-120%. Precision values expressed as relative standard deviation (RSD) were lower than 25%. Identification and confirmation of the compounds were performed by the use of retention time windows, comparison of spectra (GC-amenable compounds) or the estimation of the ion ratio (LC-amenable compounds). For GC-amenable pesticides, limits of detection (LODs) ranged from 0.001 to 0.436 μg L(-1) and limits of quantification (LOQs) from 0.003 to 1.452 μg L(-1). For LC-amenable pesticides, LODs ranged from 0.003 to 1.048 μg L(-1) and LOQs ranged from 0.011 to 3.494 μg L(-1). Finally, the optimized method was applied to the analysis of fourteen real samples of infants from agricultural population. Some pesticides such as methoxyfenozide, tebufenozide, piperonyl butoxide and propoxur were found at concentrations ranged from 1.61 to 24.4 μg L(-1), whereas methiocarb sulfoxide was detected at trace levels in two samples.
authors.affiliation: Group "Analytical Chemistry of Contaminants", Department of Analytical Chemistry, Almeria University, E-04071 Almeria, Spain.
authors.forename: Rocío
authors.initials: R
authors.lastname: Cazorla-Reyes
authors.forename: José Luis
authors.initials: JL
authors.lastname: Fernández-Moreno
authors.forename: Roberto
authors.initials: R
authors.lastname: Romero-González
authors.forename: Antonia Garrido
authors.initials: AG
authors.lastname: Frenich
authors.forename: José Luis Martínez
authors.initials: JL
authors.lastname: Vidal
mesh_terms: D000383:Agriculture; D002849:Chromatography, Gas / Q000379:methods; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D004781:Environmental Exposure / Q000032:analysis; D006801:Humans; D007231:Infant, Newborn; D057230:Limit of Detection; D010575:Pesticides / Q000032:analysis / Q000652:urine*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D010575:Pesticides