Determination of neonicotinoid insecticides residues in bovine milk samples by solid-phase extraction clean-up and liquid chromatography with diode-array detection
Autor: | Domenico Montesano, Patrizia Morrica, Paola Fidente, Serenella Seccia |
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Přispěvatelé: | Seccia, Serenella, Fidente, Paola, Montesano, Domenico, Morrica, Patrizia |
Jazyk: | angličtina |
Rok vydání: | 2008 |
Předmět: |
Insecticides
Pyridines Thiazines Food Contamination High-performance liquid chromatography Sensitivity and Specificity Biochemistry Acetamiprid Analytical Chemistry chemistry.chemical_compound Neonicotinoids Oxazines LC-DAD Animals Sample preparation Solid phase extraction Pesticides Least-Squares Analysis Insecticide Chromatography High Pressure Liquid Residue (complex analysis) Chromatography Nicotinoid Pesticide residue Solid Phase Extraction Organic Chemistry Neonicotinoid Imidazoles Pesticide Residues Reproducibility of Results General Medicine Thiacloprid Nitro Compounds Nicotinoids Pesticide Bovine milk SPE Cattle Milk Thiazoles chemistry High Pressure Liquid LC–DAD SPE Thiamethoxam |
Popis: | 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. |
Databáze: | OpenAIRE |
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