PMID- 17362971 OWN - NLM STAT- MEDLINE DCOM- 20070531 LR - 20090115 IS - 0021-9673 (Print) IS - 0021-9673 (Linking) VI - 1147 IP - 2 DP - 2007 Apr 20 TI - Analysis of carbamate and phenylurea pesticide residues in fruit juices by solid-phase microextraction and liquid chromatography-mass spectrometry. PG - 135-43 AB - A new analysis method to detect carbamates and phenylurea pesticide residues in fruit juices was developed using solid-phase microextraction (SPME) coupled with liquid chromatography-single quadrupole mass spectrometry (LC/MS) and liquid chromatography-quadrupole ion trap mass spectrometry (LC/QIT-MS). The pesticide residues present in watery matrices as fruit juices were extracted using three types of fibers: 50-microm Carbowax/templated resin (CW/TPR), 60-mum poly(dimethylsiloxane)/divinylbenzene (PDMS/DVB) and 85-microm polyacrylate. The different extraction conditions were evaluated choosing as the best parameters 90 min (time), 20 degrees C (temperature) and 1 ml (volume). After extraction, the desorption (in a static mode) was performed in the specific interface chamber SPME/HPLC, previously filled with 70% methanol and 30% water. The best recoveries, evaluated at two fortification levels (0.2 and 0.5 mg kg(-1)) in fruit juices, were obtained using PDMS/DVB and CW/TPR fibers, and ranged from 25 to 82% (monolinuron, diuron and diethofencarb), with relative standard deviations (RSDs) from 1 to 17%. All the limits of quantification (LOQs) were in the range of 0.005-0.05 microg ml(-1) and, in any case, equal to, or lower than, maximum residue limits (MRLs) established by Italian and Spanish legislations. The mass spectrometry analyses were carried out using an electrospray ionization (ESI) source operating in the positive mode both for single quadrupole and for QIT mass analysers, operating in selected ion monitoring (SIM) and in multiple reaction monitoring (MRM) modes, respectively. The proposed new method can be applied to the determination of selected pesticides in real samples of fruit juices. FAU - Sagratini, Gianni AU - Sagratini G AD - Dipartimento di Scienze Chimiche, Facolta di Farmacia, Universita di Camerino, via S.Agostino 1, 62032 Camerino, Italy. gianni.sagratini@unicam.it FAU - Manes, Jordi AU - Manes J FAU - Giardina, Dario AU - Giardina D FAU - Damiani, Pietro AU - Damiani P FAU - Pico, Yolanda AU - Pico Y LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20070224 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Carbamates) RN - 0 (Pesticide Residues) RN - 0 (Phenylurea Compounds) SB - IM MH - Beverages/*analysis MH - Carbamates/*analysis MH - Chromatography, High Pressure Liquid/*methods MH - Mass Spectrometry/*methods MH - Pesticide Residues/*analysis MH - Phenylurea Compounds/*analysis EDAT- 2007/03/17 09:00 MHDA- 2007/06/01 09:00 CRDT- 2007/03/17 09:00 PHST- 2006/12/22 00:00 [received] PHST- 2007/02/14 00:00 [revised] PHST- 2007/02/19 00:00 [accepted] PHST- 2007/03/17 09:00 [pubmed] PHST- 2007/06/01 09:00 [medline] PHST- 2007/03/17 09:00 [entrez] AID - S0021-9673(07)00363-9 [pii] AID - 10.1016/j.chroma.2007.02.066 [doi] PST - ppublish SO - J Chromatogr A. 2007 Apr 20;1147(2):135-43. doi: 10.1016/j.chroma.2007.02.066. Epub 2007 Feb 24.