title: Factorial design optimization of experimental variables in preconcentration of carbamates pesticides in water samples using solid phase extraction and liquid chromatography-electrospray-mass spectrometry determination.
abstract: An experimental design was applied for the optimization of extraction process of carbamates pesticides from surface water samples. Solid phase extraction (SPE) of carbamates compounds and their determination by liquid chromatography coupled to electrospray mass spectrometry detector were considered. A two level full factorial design 2(k) was used for selecting the variables which affected the extraction procedure. Eluent and sample volumes were statistically the most significant parameters. These significant variables were optimized using Doehlert matrix. The developed SPE method included 200mg of C-18 sorbent, 143.5 mL of water sample and 5.5 mL of acetonitrile in the elution step. For validation of the technique, accuracy, precision, detection and quantification limits, linearity, sensibility and selectivity were evaluated. Extraction recovery percentages of all the carbamates were above 90% with relative standard deviations (R.S.D.) in the range of 3-11%. The extraction method was selective and the detection and quantification limits were between 0.1 and 0.5 µg L(-1), and 1 and 3 µg L(-1), respectively.
authors.affiliation: Université de Tunis El Manar, Faculté des Sciences de Tunis, Laboratoire de Chimie Analytique et Electrochimie Campus universitaire, 2092 Tunis, Tunisie; Université de Tunis El Manar, Institut Préparatoire aux Etudes d'Ingénieurs d'El Manar, B.P.244 El Manar II, 2092 Tunis, Tunisie. Electronic address: latrous_latifa@yahoo.fr.
authors.forename: Latifa
authors.initials: L
authors.lastname: Latrous El Atrache
authors.forename: Rafika
authors.initials: R
authors.lastname: Ben Sghaier
authors.forename: Bochra
authors.initials: B
authors.lastname: Bejaoui Kefi
authors.forename: Violette
authors.initials: V
authors.lastname: Haldys
authors.forename: Mohamed
authors.initials: M
authors.lastname: Dachraoui
authors.forename: Jeanine
authors.initials: J
authors.lastname: Tortajada
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D002219:Carbamates / Q000302:isolation & purification*; D002853:Chromatography, Liquid; D005163:Factor Analysis, Statistical; D005618:Fresh Water / Q000737:chemistry*; D057230:Limit of Detection; D010575:Pesticides / Q000302:isolation & purification*; D012107:Research Design; D052616:Solid Phase Extraction; D021241:Spectrometry, Mass, Electrospray Ionization; D014874:Water Pollutants, Chemical / Q000302:isolation & purification*
chemical_list: D000097:Acetonitriles; D002219:Carbamates; D010575:Pesticides; D014874:Water Pollutants, Chemical; C032159:acetonitrile
keywords: Carbamates pesticides; Experimental design; Method validation; Solid phase extraction; Water