PMID- 22818774 OWN - NLM STAT- MEDLINE DCOM- 20121113 LR - 20120807 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1253 DP - 2012 Aug 31 TI - Dispersive liquid-liquid microextraction coupled with programmed temperature vaporization-large volume injection-gas chromatography-tandem mass spectrometry for multiclass pesticides in water. PG - 134-43 LID - 10.1016/j.chroma.2012.06.089 [doi] AB - A simple solvent-less procedure for the determination of seventeen pesticides and related compounds in environmental water and wastewater using dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry in tandem (GC-MS/MS) with large-volume injection, having a programmed temperature vaporizer (PTV-LVI), is described. The parameters affecting the extraction efficiency of the target analytes from water samples were systematically investigated. A response surface Doehlert design was used. The best extraction conditions involved a rapid injection of a mixture of 1.9 mL of acetonitrile (as a dispersant) and 178 muL of trichloroethane (as an extractant) into 10 mL of water placed in a conical bottom glass tube. After manually shaken for 3.0 min and centrifugation at 3600 rpm (5 min), 50 muL of the sedimented phase was directly injected into the PTV-LVI-GC-MS/MS system. The limits of quantitation (LOQs) ranged from 0.5 to 18 ng L(-)(1) for all pesticides, except empentrin (132 ng L(-)(1)). The relative standard deviations (RSDs) for the analytes ranged between 0.8 and 14.6% for both intraday and interday precision. Accuracy, expressed as the mean extraction recovery, was between 70 and 130%. Using the internal standard method and surrogate deuterated standards, the total concentration of pesticides was in the range from 2.7 to 440 ng L(-)(1) in seawater, river water and sewage water. CI - Copyright (c) 2012 Elsevier B.V. All rights reserved. FAU - Carro, A M AU - Carro AM AD - Dpto. de Quimica Analitica, Nutricion y Bromatologia, Facultad de Quimica, Universidad de Santiago de Compostela, Avda. de las Ciencias, s/n 15782 Santiago de Compostela, Spain. tuchi.carro@usc.es FAU - Fernandez, S AU - Fernandez S FAU - Racamonde, I AU - Racamonde I FAU - Garcia-Rodriguez, D AU - Garcia-Rodriguez D FAU - Gonzalez, P AU - Gonzalez P FAU - Lorenzo, R A AU - Lorenzo RA LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20120704 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Pesticides) RN - 0 (Sewage) RN - 0 (Water Pollutants, Chemical) SB - IM MH - Analysis of Variance MH - Gas Chromatography-Mass Spectrometry/*methods MH - Hydrogen-Ion Concentration MH - Liquid Phase Microextraction/*methods MH - Osmolar Concentration MH - Pesticides/*analysis/*isolation & purification MH - Regression Analysis MH - Reproducibility of Results MH - Seawater/chemistry MH - Sensitivity and Specificity MH - Sewage/chemistry MH - Tandem Mass Spectrometry/*methods MH - Temperature MH - Water Pollutants, Chemical/*analysis/*isolation & purification EDAT- 2012/07/24 06:00 MHDA- 2012/11/14 06:00 CRDT- 2012/07/24 06:00 PHST- 2012/03/25 00:00 [received] PHST- 2012/06/25 00:00 [revised] PHST- 2012/06/26 00:00 [accepted] PHST- 2012/07/24 06:00 [entrez] PHST- 2012/07/24 06:00 [pubmed] PHST- 2012/11/14 06:00 [medline] AID - S0021-9673(12)01009-6 [pii] AID - 10.1016/j.chroma.2012.06.089 [doi] PST - ppublish SO - J Chromatogr A. 2012 Aug 31;1253:134-43. doi: 10.1016/j.chroma.2012.06.089. Epub 2012 Jul 4.