PMID- 19071541 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20091216 LR - 20081216 IS - 1873-3573 (Electronic) IS - 0039-9140 (Linking) VI - 71 IP - 5 DP - 2007 Mar 30 TI - Gas chromatography mass spectrometry determination of acaricides from honey after a new fast ultrasonic-based solid phase micro-extraction sample treatment. PG - 1906-14 LID - 10.1016/j.talanta.2006.08.035 [doi] AB - A method is reported for the determination of acaricides (amitraz, bromopropylate, coumaphos and fluvalinate) from honey by gas chromatography mass spectrometry after a new fast solid phase micro-extraction, SPME, procedure. Six different fibers were assessed for micro-extraction purpose studying the following variables: (i) SPME coating, (ii) extraction temperature, (iii) extraction time, (iv) desorption conditions and (v) agitation conditions. The new ultrasonic bath technology providing different sonication frequencies (35 and 130kHz) and different working modes (Sweep, Standard and Degas) was studied and optimized for speeding up the acaricide micro-extraction. The best extraction results were achieved with the polyacrylate fiber. The extraction process was done in 30min using the ultrasonic bath at 130kHz in the Standard mode. Quality parameters of the proposed method show a good precision (<11%) and detection and quantitation limits lower than 6 and 15ng/g, respectively, except for fluvalinate. Eleven Portuguese commercial honey samples were analyzed with the developed method in order to assess the performance of the method with real samples and to determine whether the concentration of acaricides in honey exceed their maximum residue levels (MRLs). Acaricide residues detected were lower than those established by the legislation. FAU - Rial-Otero, R AU - Rial-Otero R AD - REQUIMTE, Departamento de Quimica, Faculdade de Ciencias e Tecnologia, Universidade Nova de Lisboa, 2829-516 Monte de Caparica, Portugal. raquelrial@dq.fct.unl.pt FAU - Gaspar, E M AU - Gaspar EM FAU - Moura, I AU - Moura I FAU - Capelo, J L AU - Capelo JL LA - eng PT - Journal Article DEP - 20060925 PL - Netherlands TA - Talanta JT - Talanta JID - 2984816R EDAT- 2007/03/30 00:00 MHDA- 2007/03/30 00:01 CRDT- 2008/12/17 09:00 PHST- 2006/06/16 00:00 [received] PHST- 2006/08/20 00:00 [revised] PHST- 2006/08/21 00:00 [accepted] PHST- 2008/12/17 09:00 [entrez] PHST- 2007/03/30 00:00 [pubmed] PHST- 2007/03/30 00:01 [medline] AID - S0039-9140(06)00597-2 [pii] AID - 10.1016/j.talanta.2006.08.035 [doi] PST - ppublish SO - Talanta. 2007 Mar 30;71(5):1906-14. doi: 10.1016/j.talanta.2006.08.035. Epub 2006 Sep 25.