PMID- 18952214 OWN - NLM STAT- MEDLINE DCOM- 20090511 LR - 20090316 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1216 IP - 14 DP - 2009 Apr 3 TI - Development of a matrix solid-phase dispersion method for the simultaneous determination of pyrethroid and organochlorinated pesticides in cattle feed. PG - 2832-42 LID - 10.1016/j.chroma.2008.10.026 [doi] AB - A matrix solid-phase dispersion (MSPD) method was developed for the simultaneous extraction of 36 common pesticides and breakdown products (mostly pyrethroids and organochlorines) in cattle feed. Different parameters affecting the extraction efficiency (such as dispersing phase, clean-up adsorbent and elution volume) were investigated. The experimental procedure was optimized using a multivariate statistical approach and the final analyses were carried out by GC-muECD. Several protocols for extract purification were also studied. As far as we know, this is the first application of MSPD for the extraction of most of the target pesticides from animal feed. Using the optimized extraction conditions, the method was validated in terms of accuracy, and precision (within-a-day and among-days), using a certified reference material (CRM 115) as well as spiked cattle feedingstuffs at different concentration levels. A matrix effect study was also carried out using various real samples. The recoveries were satisfactory (>75% in most cases) and the quantification limits, at the sub-ngg(-1) or low-ngg(-1) level, complied with the regulated maximum residue levels (MRLs) in animal feed and in main crops used in the preparation of cattle feeding materials. Finally, the MSPD-GC-muECD methodology was applied to the analysis of real cattle feed samples collected in farms of dairy cattle from NW Spain. FAU - Fernandez-Alvarez, Maria AU - Fernandez-Alvarez M AD - Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain. FAU - Llompart, Maria AU - Llompart M FAU - Lamas, J Pablo AU - Lamas JP FAU - Lores, Marta AU - Lores M FAU - Garcia-Jares, Carmen AU - Garcia-Jares C FAU - Cela, Rafael AU - Cela R FAU - Dagnac, Thierry AU - Dagnac T LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20081014 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Pesticide Residues) RN - 0 (Pyrethrins) SB - IM MH - Animal Feed/*analysis MH - Animals MH - Cattle MH - Chromatography, Gas/*methods MH - Food Contamination/*analysis MH - Pesticide Residues/*analysis MH - Pyrethrins/*analysis MH - Solid Phase Extraction/*methods EDAT- 2008/10/28 09:00 MHDA- 2009/05/12 09:00 CRDT- 2008/10/28 09:00 PHST- 2008/07/07 00:00 [received] PHST- 2008/10/01 00:00 [revised] PHST- 2008/10/08 00:00 [accepted] PHST- 2008/10/28 09:00 [pubmed] PHST- 2009/05/12 09:00 [medline] PHST- 2008/10/28 09:00 [entrez] AID - S0021-9673(08)01766-4 [pii] AID - 10.1016/j.chroma.2008.10.026 [doi] PST - ppublish SO - J Chromatogr A. 2009 Apr 3;1216(14):2832-42. doi: 10.1016/j.chroma.2008.10.026. Epub 2008 Oct 14.