title: Application of solid-phase extraction and liquid chromatography-mass spectrometry to the determination of neonicotinoid pesticide residues in fruit and vegetables.
abstract: A rapid and simple method for simultaneous analysis of four neonicotinoid insecticides including acetamiprid, imidacloprid, thiacloprid and thiamethoxam in fruit and vegetable matrices has been developed. For instance, ready-to-use cartridges filled with a macroporous diatomaceous material were used to extract in a single step insecticide residues with dichloromethane from aqueous-acetone extracts of fruits and vegetables. The eluate was evaporated, the residue redissolved with methanol and then analyzed by liquid chromatography-mass spectrometry in the electrospray ionization (ESI) positive mode. Average recoveries of the four pesticides were between 74.5 and 105% at both spiking levels 0.1 and 1.0 mg kg(-1) in peach, pear, courgette, celery and apricot. Relative standard deviations (RSDs) were less than 10% for all of the recovery tests. The calculated limits of quantitation (LOQs) (0.1-0.5 mg kg(-1)) were equal or lower then the maximum residue limits (MRLs) established by European legislation (0.1-0.5 mg kg(-1)). The proposed method is fast, easy to perform and could be utilized for monitoring of pesticides residues.
authors.affiliation: ISS Istituto Superiore di Sanità (National Institute of Health), Viale Regina Elena 299, 00161 Rome, Italy.
authors.forename: Alfonso
authors.initials: A
authors.lastname: Di Muccio
authors.forename: Paola
authors.initials: P
authors.lastname: Fidente
authors.forename: Danilo Attard
authors.initials: DA
authors.lastname: Barbini
authors.forename: Roberto
authors.initials: R
authors.lastname: Dommarco
authors.forename: Serenella
authors.initials: S
authors.lastname: Seccia
authors.forename: Patrizia
authors.initials: P
authors.lastname: Morrica
mesh_terms: D005591:Chemical Fractionation / Q000379:methods*; D002853:Chromatography, Liquid / Q000379:methods; D005638:Fruit / Q000737:chemistry*; D007093:Imidazoles / Q000032:analysis; D007306:Insecticides / Q000032:analysis*; D000073943:Neonicotinoids; D009574:Nitro Compounds / Q000032:analysis; D010078:Oxazines / Q000032:analysis; D010573:Pesticide Residues / Q000032:analysis*; D011725:Pyridines / Q000032:analysis; D015203:Reproducibility of Results; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D000077922:Thiamethoxam; D013843:Thiazines / Q000032:analysis; D013844:Thiazoles; D014675:Vegetables / Q000737:chemistry*
chemical_list: D007093:Imidazoles; D007306:Insecticides; D000073943:Neonicotinoids; D009574:Nitro Compounds; D010078:Oxazines; D010573:Pesticide Residues; D011725:Pyridines; D013843:Thiazines; D013844:Thiazoles; C082359:imidacloprid; C464485:acetamiprid; D000077922:Thiamethoxam; C417209:thiacloprid