title: Development and validation of a solid-phase extraction method coupled to high-performance liquid chromatography with ultraviolet-diode array detection for the determination of sulfonylurea herbicide residues in bovine milk samples.
abstract: This study proposes a fast, simple and sensitive liquid chromatography diode array detector (LC/UV-DAD)-based method for the simultaneous determination of eight sulfonylurea herbicides (bensulfuron methyl, chlorsulfuron, metsulfuron methyl, primisulfuron methyl, rimsulfuron, thifensulfuron methyl, triasulfuron and tribenuron methyl) in bovine whole milk at concentrations lower than the default limit of 0.01 mg kg(-1) allowed by current legislation (Regulation EC/396/2005 and following Annexes). An effective one-step solid phase extraction (SPE) and clean up procedure was defined with use of Chem Elut cartridges, providing good recoveries for all the analytes tested and with no matrix effects affecting method accuracy. Separation of herbicides was obtained on a C(18) column by acetonitrile- water gradient elution. Method validation has been performed according to European Commission Decision 2002/657/EC criteria, in terms of linearity, recovery, precision, specificity, decision limit (CC(α)) and detection capability (CC(β)). Typical recoveries ranged between 78.4% and 99.7%, at the maximum residue limits (MRLs) levels established by Regulation EC/396/2005, with relative standard deviations (RSD) no larger than 10%.
authors.affiliation: Dipartimento di Chimica Farmaceutica e Tossicologica, Università degli Studi di Napoli Federico II, Via D. Montesano 49, 80131 Napoli, Italy. seccia@unina.it
authors.forename: Serenella
authors.initials: S
authors.lastname: Seccia
authors.forename: Stefania
authors.initials: S
authors.lastname: Albrizio
authors.forename: Paola
authors.initials: P
authors.lastname: Fidente
authors.forename: Domenico
authors.initials: D
authors.lastname: Montesano
mesh_terms: D000818:Animals; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis* / Q000302:isolation & purification; D006540:Herbicides / Q000032:analysis* / Q000302:isolation & purification; D016018:Least-Squares Analysis; D008892:Milk / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*; D013056:Spectrophotometry, Ultraviolet; D013453:Sulfonylurea Compounds / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D006540:Herbicides; D013453:Sulfonylurea Compounds