Application of ultrasound-assisted emulsification-micro-extraction for the analysis of organochlorine pesticides in waters.

Ultrasound-assisted emulsification-micro-extraction (USAEME) procedure was developed for the determination of different organochlorine pesticides (OCPs) in water samples by gas chromatography with mu-electron capture detection (GC-microECD). After the determination of the most suitable extraction solvent and its volume, parameters such as extraction time, centrifugation time and ionic strength of the sample were optimized by using a 2(3) factorial experimental design. For 10 mL of water sample, the optimized USAEME procedure used 200 microL of chloroform as extraction solvent, 15 min of extraction without ionic strength adjustment at 25 degrees C and 5 min of centrifugation at 4000 rpm. Limits of detection ranged from 0.002 to 0.016 microg L(-1). Mean recoveries of OCPs from fortified water samples are over 96% for three different fortification levels between 0.5 and 5 microg L(-1) and relative standard deviations of the recoveries are below 9%. The developed procedure was successfully applied for real water samples (i.e., tap water, well water, surface (lake) water, domestic and industrial wastewater). Performance of the procedure was compared with those involving traditional liquid-liquid extraction and solid-phase extraction. The result demonstrates that the USAEME procedure is viable, rapid and easy to use for analysis of OCPs in water samples.

[1]  Rafael Cela,et al.  Ultrasound-assisted emulsification-microextraction of emergent contaminants and pesticides in environmental waters. , 2008, Journal of chromatography. A.

[2]  O. Fatoki,et al.  Methods for selective determination of persistent organochlorine pesticide residues in water and sediments by capillary gas chromatography and electron-capture detection. , 2003, Journal of chromatography. A.

[3]  A. Tor,et al.  Application of liquid-phase microextraction to the analysis of trihalomethanes in water. , 2006, Analytica chimica acta.

[4]  B. Tomkins,et al.  Determination of organochlorine pesticides in ground water using solid-phase microextraction followed by dual-column gas chromatography with electron-capture detection. , 2002, Journal of chromatography. A.

[5]  S. Igarashi,et al.  Powerful preconcentration method for capillary electrophoresis and its application to analysis of ultratrace amounts of polycyclic aromatic hydrocarbons , 2006, Analytical and bioanalytical chemistry.

[6]  Senar Ozcan,et al.  Ultrasonic solvent extraction of organochlorine pesticides from soil , 2006 .

[7]  A. Tor.  Determination of chlorobenzenes in water by drop-based liquid-phase microextraction and gas chromatography-electron capture detection. , 2006, Journal of chromatography. A.

[8]  M. Anbia,et al.  Dispersive liquid-liquid microextraction combined with gas chromatography-flame photometric detection. Very simple, rapid and sensitive method for the determination of organophosphorus pesticides in water. , 2006, Journal of chromatography. A.

[9]  F. Borrull,et al.  Determination of pesticides in environmental waters by solid-phase extraction and gas chromatography with electron-capture and mass spectrometry detection , 1997 .

[10]  V. Vickackaite,et al.  Headspace extraction of alcohols into a single drop , 2001 .

[11]  J. Hernández-Méndez,et al.  Cloud point extraction as a preconcentration step prior to capillary electrophoresis. , 1999, Analytical chemistry.

[12]  A. Tor,et al.  Determination of selected polychlorinated biphenyls in soil by miniaturised ultrasonic solvent extraction and gas chromatography-mass-selective detection. , 2006, Analytica chimica acta.

[13]  F. Priego-Capote,et al.  Ultrasound-assisted preparation of liquid samples. , 2007, Talanta.

[14]  D. Barceló.  Environmental Protection Agency and other methods for the determination of priority pesticides and their transformation products in water , 1993 .

[15]  M. D. Luque de Castro,et al.  Ultrasound-assisted derivatization of phenolic compounds in spiked water samples before pervaporation, gas chromatographic separation, and flame lonization detection , 2003 .

[16]  Hian Kee Lee,et al.  Application of static liquid-phase microextraction to the analysis of organochlorine pesticides in water. , 2001, Journal of chromatography. A.

[17]  L. D. de Jager,et al.  Development of a rapid screening technique for organochlorine pesticides using solvent microextraction (SME) and fast gas chromatography (GC). , 2000, The Analyst.

[18]  L. Martínez,et al.  Simple approach based on ultrasound-assisted emulsification-microextraction for determination of polibrominated flame retardants in water samples by gas chromatography-mass spectrometry. , 2009, Journal of chromatography. A.

[19]  Z. Zeng,et al.  Determination of organochlorine pesticides and their derivations in water after HS-SPME using polymethylphenylvinylsiloxane-coated fiber by GC-ECD. , 2005, Water research.

[20]  F. Rezaei,et al.  Development of a dispersive liquid-liquid microextraction method for the determination of polychlorinated biphenyls in water. , 2008, Journal of hazardous materials.

[21]  N. Kalogerakis,et al.  Headspace single-drop microextraction for the analysis of chlorobenzenes in water samples. , 2005, Journal of chromatography. A.

[22]  J. Jen,et al.  Determination of organochlorine pesticides in water using microwave assisted headspace solid-phase microextraction and gas chromatography. , 2003, Journal of chromatography. A.

[23]  M. D. Luque de Castro,et al.  Analytical Applications of Ultrasound , 2007 .

[24]  B. Page,et al.  Application of solid-phase microextraction to the headspace gas chromatographic analysis of semi-volatile organochlorine contaminants in aqueous matrices , 1997 .

[25]  A. Tor,et al.  Application of miniaturised ultrasonic extraction to the analysis of organochlorine pesticides in soil. , 2009, Analytica Chimica Acta.

[26]  T. Mason,et al.  Applied Sonochemistry: The Uses of Power Ultrasound in Chemistry and Processing , 2002 .

[27]  Nicolas Kalogerakis,et al.  Developments in liquid-phase microextraction , 2003 .

[28]  F. Borrull,et al.  Determination of organophosphorus pesticides in environmental water samples using GC-MS and two membrane extraction disks , 1996 .

[29]  S. Pedersen‐Bjergaard,et al.  Developments in hollow fibre-based, liquid-phase microextraction , 2004 .

[30]  Patricia Boone,et al.  QA/QC Guidance for Sampling and Analysis of Sediments, Water, and Tissues for Dredged Material Evaluations: Chemical Evaluations , 1995 .

[31]  Alicia Romo,et al.  Determination of organochlorine pesticides in complex matrices by single-drop microextraction coupled to gas chromatography-mass spectrometry. , 2009, Analytica chimica acta.

[32]  M. Rezaee,et al.  Determination of organic compounds in water using dispersive liquid-liquid microextraction. , 2006, Journal of chromatography. A.

[33]  S. Pedersen‐Bjergaard,et al.  Liquid-phase microextraction of protein-bound drugs under non-equilibrium conditions. , 2002, The Analyst.

[34]  Xiao-bai Xu,et al.  Headspace liquid-phase microextraction of trihalomethanes in drinking water and their gas chromatographic determination. , 2004, Talanta.