title: Selective extraction and determination of neonicotinoid insecticides in wine by liquid chromatography-tandem mass spectrometry.
abstract: A simplified, high throughput procedure for the determination of five neonicotinoid insecticides in red and white wines, using liquid chromatography (LC)-tandem mass spectrometry (MS/MS), is presented. The effects of different experimental parameters (extraction sorbent, solvent elution and clean-up conditions) in the efficiency and the selectivity of the sample preparation process were assessed through calculation of the extraction yields and the matrix effects (MEs). Wines (10mL) were concentrated using OASIS HLB cartridges, on-line connected to Florisil clean-up cartridges, with acetonitrile serving as the elution solvent. The extract (5mLvol) was concentrated to 1mL and injected in the LC-ESI-MS/MS system. The optimized procedure provided quantitative extraction yields at the same time that the efficiency of ESI ionization remained unchanged between standards and sample extracts. Overall recoveries, calculated against authentic standards in ACN, varied between 77 and 119% and the attained limits of quantification remained below 0.2ngmL(-1). Analysis of commercial wines revealed imidacloprid residues in more than 50% of processed samples, with a maximum level of 14ngmL(-1).
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
authors.forename: T
authors.initials: T
authors.lastname: Rodríguez-Cabo
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
authors.forename: J
authors.initials: J
authors.lastname: Casado
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain. Electronic address: isaac.rodriguez@usc.es.
authors.forename: I
authors.initials: I
authors.lastname: Rodríguez
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
authors.forename: M
authors.initials: M
authors.lastname: Ramil
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Instituto de Investigación y Análisis Alimentario (IIAA), Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain.
authors.forename: R
authors.initials: R
authors.lastname: Cela
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D002853:Chromatography, Liquid; D005504:Food Analysis / Q000379:methods*; D007093:Imidazoles / Q000032:analysis; D007306:Insecticides / Q000032:analysis*; D057230:Limit of Detection; D000073943:Neonicotinoids; D009574:Nitro Compounds / Q000032:analysis; D053719:Tandem Mass Spectrometry; D014920:Wine / Q000032:analysis*
chemical_list: D000097:Acetonitriles; D007093:Imidazoles; D007306:Insecticides; D000073943:Neonicotinoids; D009574:Nitro Compounds; C082359:imidacloprid; C032159:acetonitrile
keywords: Liquid chromatography–tandem mass spectrometry; Neonicotinoids; Solid-phase extraction; Wine analysis