PMID- 19004450 OWN - NLM STAT- MEDLINE DCOM- 20090219 LR - 20181201 IS - 0021-9673 (Print) IS - 0021-9673 (Linking) VI - 1214 IP - 1-2 DP - 2008 Dec 19 TI - Determination of neonicotinoid insecticides residues in bovine milk samples by solid-phase extraction clean-up and liquid chromatography with diode-array detection. PG - 115-20 LID - 10.1016/j.chroma.2008.10.088 [doi] AB - 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. FAU - Seccia, Serenella AU - Seccia S AD - Dipartimento di Chimica Farmaceutica e Tossicologica, Universita degli Studi di Napoli Federico II, Via D. Montesano 49, 80131 Naples, Italy. seccia@unina.it FAU - Fidente, Paola AU - Fidente P FAU - Montesano, Domenico AU - Montesano D FAU - Morrica, Patrizia AU - Morrica P LA - eng PT - Journal Article DEP - 20081030 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Imidazoles) RN - 0 (Insecticides) RN - 0 (Neonicotinoids) RN - 0 (Nitro Compounds) RN - 0 (Oxazines) RN - 0 (Pesticide Residues) RN - 0 (Pyridines) RN - 0 (Thiazines) RN - 0 (Thiazoles) RN - 3BN7M937V8 (imidacloprid) RN - 5HL5N372P0 (acetamiprid) RN - 747IC8B487 (Thiamethoxam) RN - DSV3A944A4 (thiacloprid) SB - IM MH - Animals MH - Cattle MH - Chromatography, High Pressure Liquid/*methods MH - Food Contamination/*analysis MH - Imidazoles/analysis MH - Insecticides/*analysis MH - Least-Squares Analysis MH - Milk/*chemistry MH - Neonicotinoids MH - Nitro Compounds/analysis MH - Oxazines/analysis MH - Pesticide Residues/*analysis MH - Pyridines/analysis MH - Reproducibility of Results MH - Sensitivity and Specificity MH - *Solid Phase Extraction MH - Thiamethoxam MH - Thiazines/analysis MH - Thiazoles/analysis EDAT- 2008/11/14 09:00 MHDA- 2009/02/20 09:00 CRDT- 2008/11/14 09:00 PHST- 2008/07/01 00:00 [received] PHST- 2008/10/02 00:00 [revised] PHST- 2008/10/24 00:00 [accepted] PHST- 2008/11/14 09:00 [pubmed] PHST- 2009/02/20 09:00 [medline] PHST- 2008/11/14 09:00 [entrez] AID - S0021-9673(08)01884-0 [pii] AID - 10.1016/j.chroma.2008.10.088 [doi] PST - ppublish SO - J Chromatogr A. 2008 Dec 19;1214(1-2):115-20. doi: 10.1016/j.chroma.2008.10.088. Epub 2008 Oct 30.