PMID- 18501913 OWN - NLM STAT- MEDLINE DCOM- 20080902 LR - 20131121 IS - 0021-9673 (Print) IS - 0021-9673 (Linking) VI - 1195 IP - 1-2 DP - 2008 Jun 27 TI - Single-drop coacervative microextraction of organic compounds prior to liquid chromatography. Theoretical and practical considerations. PG - 25-33 LID - 10.1016/j.chroma.2008.05.002 [doi] AB - Coacervates made of surfactant aggregates, namely aqueous and reverse micelles and vesicles, were firstly used as solvents in single-drop microextraction (SDME) and proposed for the extraction and concentration of chlorophenols prior to liquid chromatography. The formation of coacervate drops in the needle tip of conventional microsyringes depended on the type of intermolecular forces established between the surfactant headgroups making up the supramolecular aggregates; hydrogen bond interactions were strong enough to permit the formation of spherical drops. Stability of 1-50 microL coacervate drops was achieved by introducing the microsyringe needle tip in a PTFE rod, the end of which had been machined out with a heated flanging-tool to get circular flanges (diameters in the range 3.5-6 mm). The parameters affecting the efficiency of single-drop coacervative microextraction (SDCME) were investigated using vesicular coacervates as a solvent and 2-chlorophenol (CP), 2,4-dichlorophenol (DCP), 2,4,6-trichlorophenol (TCP) and pentachlorophenol (PCP) as model analytes. Coacervative microextraction dynamics fit to the general rate equation of liquid-liquid extraction. The effect of variables such as extraction time, drop volume, stirring rate, pH and temperature, on the extraction of chlorophenols was similar to that described for organic solvent drops. Electrolyte concentrations above 0.1 M caused drop instability. Under the optimum conditions, detection limits were in the range 0.1-0.3 microg L(-1). The relative standard deviation was between 4.3 and 5.6 at 20 microg L(-1) spiked level. The method was applied to the determination of the four chlorophenols in wastewater, superficial water from a reservoir and groundwater and the recoveries were in the range 79 and 106% at 5-20 microg L(-1) spiked level. FAU - Lopez-Jimenez, Francisco Jose AU - Lopez-Jimenez FJ AD - Departamento de Quimica Analitica, Universidad de Cordoba, Edificio Marie Curie (Anexo), Campus Universitario de Rabanales, E-14071 Cordoba, Spain. FAU - Rubio, Soledad AU - Rubio S FAU - Perez-Bendito, Dolores AU - Perez-Bendito D LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20080510 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Chlorophenols) RN - 0 (Organic Chemicals) RN - 0 (Water Pollutants, Chemical) RN - D9BSU0SE4T (Pentachlorophenol) RN - K9KAV4K6BN (2-chlorophenol) RN - MHS8C5BAUZ (2,4,6-trichlorophenol) RN - R669TG1950 (2,4-dichlorophenol) SB - IM MH - Chemical Fractionation/instrumentation/*methods MH - Chlorophenols/isolation & purification MH - Chromatography, Liquid/*methods MH - Organic Chemicals/*isolation & purification MH - Pentachlorophenol/isolation & purification MH - Reproducibility of Results MH - Water Pollutants, Chemical/isolation & purification EDAT- 2008/05/27 09:00 MHDA- 2008/09/03 09:00 CRDT- 2008/05/27 09:00 PHST- 2007/07/20 00:00 [received] PHST- 2008/03/19 00:00 [revised] PHST- 2008/05/07 00:00 [accepted] PHST- 2008/05/27 09:00 [pubmed] PHST- 2008/09/03 09:00 [medline] PHST- 2008/05/27 09:00 [entrez] AID - S0021-9673(08)00827-3 [pii] AID - 10.1016/j.chroma.2008.05.002 [doi] PST - ppublish SO - J Chromatogr A. 2008 Jun 27;1195(1-2):25-33. doi: 10.1016/j.chroma.2008.05.002. Epub 2008 May 10.