title: Determination of neonicotinoid insecticides residues in bovine milk samples by solid-phase extraction clean-up and liquid chromatography with diode-array detection.
abstract: In this paper we have developed an analytical method for the simultaneous determination of four nicotinoid insecticides [acetamiprid (ACT), imidacloprid (ICL), thiacloprid (TCL) and thiamethoxam (TMX)] in bovine whole milk. These analytes were extracted, in a single step with dichloromethane, from fortified milk samples, using Chem Elut cartridges, containing diatomaceous earth material. Insecticide's determination and quantification were performed by HPLC with diode-array detection (DAD). Average recoveries of the four insecticides from bovine milk samples were between 85.1 and 99.7% at spiking levels 0.01, 0.05 and 0.1 mg kg(-1). Relative standard deviations (RSDs) were no larger than 10% for all of the recovery tests. The calculated limits of quantitation (LOQ) ranged from 0.01 to 0.04 mg kg(-1) for the four insecticides, being equal to or lower than the maximum residue limits (MRLs) established by European legislation (0.01-0.05 mg kg(-1)). The developed method is linear at concentrations within the tested interval, with coefficients of determination higher than 0.9990. According to Commission Decision 2002/657/EC, decision limit (CCalpha) and detection capability (CCbeta) have been calculated. The proposed method is rapid, simple and could be utilized for the routine analysis of pesticides residues.
authors.affiliation: Dipartimento di Chimica Farmaceutica e Tossicologica, Università degli Studi di Napoli Federico II, Via D. Montesano 49, 80131 Naples, Italy. seccia@unina.it
authors.forename: Serenella
authors.initials: S
authors.lastname: Seccia
authors.forename: Paola
authors.initials: P
authors.lastname: Fidente
authors.forename: Domenico
authors.initials: D
authors.lastname: Montesano
authors.forename: Patrizia
authors.initials: P
authors.lastname: Morrica
mesh_terms: D000818:Animals; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D007093:Imidazoles / Q000032:analysis; D007306:Insecticides / Q000032:analysis*; D016018:Least-Squares Analysis; D008892:Milk / Q000737:chemistry*; D000073943:Neonicotinoids; D009574:Nitro Compounds / Q000032:analysis; D010078:Oxazines / Q000032:analysis; D010573:Pesticide Residues / Q000032:analysis*; D011725:Pyridines / Q000032:analysis; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction; D000077922:Thiamethoxam; D013843:Thiazines / Q000032:analysis; D013844:Thiazoles / Q000032:analysis
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