title: Liquid chromatography quadrupole time-of-flight mass spectrometry selective determination of ochratoxin A in wine.
abstract: The performance of liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) for ochratoxin A (OTA) determination in wine is evaluated for the first time. Sample preparation was optimized to obtain quantitative recoveries at the same time that the efficiency of electrospray ionization (ESI) remained unaltered between sample extracts and calibration standards. Under final conditions, samples (20 mL) were concentrated using a reversed-phase solid-phase extraction (SPE) cartridge, followed by OTA elution with 1 mL of ethyl acetate. The absolute recoveries of the method, established against calibration standards, were 91-121% and 90-113% (without and with internal standard correction, respectively), for wines fortified at 3 concentration levels. The attained LOQ (0.05 ng mL(-1)) remained below the maximum permitted OTA concentration (2 ng mL(-1)) in dry wines. The method was applied to different samples, with OTA being found in some dessert wines at concentrations below 1 ng mL(-1). The ethyl ester of OTA (OTC) could be identified in the same wine samples from its accurate full product ion spectra.
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. 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: D002853:Chromatography, Liquid / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods*; D009793:Ochratoxins / Q000032:analysis / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D014920:Wine / Q000032:analysis*
chemical_list: D009793:Ochratoxins; C025589:ochratoxin A
keywords: Liquid chromatography quadrupole time-of-flight mass spectrometry; Ochratoxin A; Solid-phase extraction; Wine