title: Determination of spirocyclic tetronic/tetramic acid derivatives and neonicotinoid insecticides in fruits and vegetables by liquid chromatography and mass spectrometry after dispersive liquid-liquid microextraction.
abstract: Dispersive liquid-liquid microextraction was used to preconcentrate three spirocyclic tetronic/tetramic acid derivatives (spirotetramat, spiromesifen and spirodiclofen) and five neonicotinoid (thiamethoxam, chlotianidin, imidacloprid, acetamiprid and thiacloprid) insecticides previously extracted from fruit and vegetable matrices with acetonitrile. The organic enriched phase was evaporated, reconstituted in 25μL acetonitrile and analyzed by reversed-phase liquid chromatography with tandem mass spectrometry using a triple quadrupole in selected reaction monitoring mode. Enrichment factors in the 15-100 range were obtained. A matrix effect was observed, the detection limits varying between 0.025 and 0.5ngg(-1), depending on the compound and the sample matrix. The developed method was applied to the analysis of 25 samples corresponding to five different fruit and vegetable matrices. Only thiamethoxam was detected in a lemon sample at a concentration close to the quantification limit, and spiromesifen and spirotetramat at concentrations between 11.6 and 54.5ngg(-1).
authors.affiliation: Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence "Campus Mare Nostrum", University of Murcia, E-30100 Murcia, Spain.
authors.forename: Marta
authors.initials: M
authors.lastname: Pastor-Belda
authors.affiliation: Equipo de Calidad Alimentaria, Instituto Murciano de Investigación y Desarrollo Agrario y Alimentario (IMIDA), C/ Mayor s/n, La Alberca, 30150 Murcia, Spain.
authors.forename: Isabel
authors.initials: I
authors.lastname: Garrido
authors.affiliation: Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence "Campus Mare Nostrum", University of Murcia, E-30100 Murcia, Spain.
authors.forename: Natalia
authors.initials: N
authors.lastname: Campillo
authors.affiliation: Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence "Campus Mare Nostrum", University of Murcia, E-30100 Murcia, Spain.
authors.forename: Pilar
authors.initials: P
authors.lastname: Viñas
authors.affiliation: Equipo de Calidad Alimentaria, Instituto Murciano de Investigación y Desarrollo Agrario y Alimentario (IMIDA), C/ Mayor s/n, La Alberca, 30150 Murcia, Spain.
authors.forename: Pilar
authors.initials: P
authors.lastname: Hellín
authors.affiliation: Equipo de Calidad Alimentaria, Instituto Murciano de Investigación y Desarrollo Agrario y Alimentario (IMIDA), C/ Mayor s/n, La Alberca, 30150 Murcia, Spain.
authors.forename: Pilar
authors.initials: P
authors.lastname: Flores
authors.affiliation: Equipo de Calidad Alimentaria, Instituto Murciano de Investigación y Desarrollo Agrario y Alimentario (IMIDA), C/ Mayor s/n, La Alberca, 30150 Murcia, Spain. Electronic address: jose.fenoll@carm.es.
authors.forename: José
authors.initials: J
authors.lastname: Fenoll
mesh_terms: D002851:Chromatography, High Pressure Liquid; D005638:Fruit / Q000737:chemistry*; D007306:Insecticides / Q000032:analysis*; D059627:Liquid Phase Microextraction / Q000379:methods*; D000073943:Neonicotinoids; D009574:Nitro Compounds / Q000032:analysis; D010078:Oxazines / Q000032:analysis; D011760:Pyrrolidinones / Q000032:analysis; D021241:Spectrometry, Mass, Electrospray Ionization; D000077922:Thiamethoxam; D013844:Thiazoles / Q000032:analysis; D014675:Vegetables / Q000737:chemistry*
chemical_list: D007306:Insecticides; D000073943:Neonicotinoids; D009574:Nitro Compounds; D010078:Oxazines; D011760:Pyrrolidinones; D013844:Thiazoles; C009435:tetramic acid; D000077922:Thiamethoxam
keywords: Dispersive liquid–liquid microextraction; Fruits; Insecticides; Liquid chromatography–tandem mass spectrometry; Neonicotinoids; Spirocyclic tetronic/tetramic acid derivatives; Vegetables