Ultrasound-assisted emulsification-microextraction of emergent contaminants and pesticides in environmental waters.

The analytical use of ultrasound-generated emulsions has recently found a growing interest to improve efficiency in liquid-liquid extraction since they increase the speed of the mass transfer between the two immiscible phases implied. Thus, dispersed droplets can act as efficient liquid-liquid microextractors in the continuous phase, and later they can be readily separated by centrifugation. A novel method based on ultrasound-assisted emulsification-microextraction (USAEME) and gas chromatography coupled to mass spectrometry (GC/MS) has been developed for the analysis of synthetic musk fragrances, phthalate esters and lindane in water samples. Extraction conditions were optimized using a multivariate approach. Compounds were extracted during 10 min in an acoustically emulsified media formed by 100 microL chloroform and 10 mL sample (enrichment factor=100). The method performance was studied in terms of accuracy (recovery=78-114%), linearity (R2> or =0.9990) and repeatability (RSD< or =14%). Limits of detection (LODs) were at the pg mL(-1) level for most of compounds, and at the sub-ng mL(-1) level for the most ubiquitous phthalate esters. USAEME is proposed as an efficient, fast, simple and non-expensive alternative to other extraction techniques such as SPE, SPME and LPME for the analysis of environmental waters including bottled, tap, river, municipal swimming pool, sewage and seaport water samples. Since no matrix effect has been found for any of the water types analyzed, quantification could be carried out by using conventional external calibration, thus allowing a higher throughput of the analysis in comparison with other microextraction techniques based on equilibrium such as solid-phase microextraction.

[1]  R. Cela,et al.  Multivariate optimization of a solid-phase microextraction method for the analysis of phthalate esters in environmental waters. , 2005, Journal of chromatography. A.

[2]  H. S. Fogler,et al.  Emulsion stability of acoustically formed emulsions , 1980 .

[3]  J. S. Gándara,et al.  Multiresidue method for fourteen fungicides in white grapes by liquid-liquid and solid-phase extraction followed by liquid chromatography-diode array detection. , 2003 .

[4]  Dennis R. Peterson,et al.  The environmental fate of phthalate esters: A literature review , 1997 .

[5]  T. Ternes,et al.  Pharmaceuticals and personal care products in the environment: agents of subtle change? , 1999, Environmental health perspectives.

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

[7]  M. Povey,et al.  The application of modified forms of the Urick equation to the interpretation of ultrasound velocity in scattering systems , 1995 .

[8]  Rafael Cela,et al.  Optimisation of a solid-phase microextraction method for synthetic musk compounds in water. , 2002, Journal of chromatography. A.

[9]  N. Lawrence,et al.  Ultrasonic extraction of iron from non-aqueous liquids. , 2002, The Analyst.

[10]  N. Kalogerakis,et al.  Hollow-fibre liquid-phase microextraction of phthalate esters from water. , 2003, Journal of chromatography. A.

[11]  G G Rimkus,et al.  Polycyclic musk fragrances in the aquatic environment. , 1999, Toxicology letters.

[12]  R. Cela,et al.  Multivariate optimization of the factors influencing the solid-phase microextraction of pyrethroid pesticides in water. , 2006, Journal of chromatography. A.

[13]  Rafael Cela,et al.  Optimization of a sensitive method for the determination of nitro musk fragrances in waters by solid-phase microextraction and gas chromatography with micro electron capture detection using factorial experimental design , 2007, Analytical and bioanalytical chemistry.

[14]  R. Cela,et al.  Development of a sensitive methodology for the analysis of chlorobenzenes in air by combination of solid-phase extraction and headspace solid-phase microextraction. , 2004, Journal of chromatography. A.

[15]  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.

[16]  J. Pawliszyn,et al.  Solid phase microextraction with thermal desorption using fused silica optical fibers , 1990 .

[17]  Hian Kee Lee,et al.  Determination of pesticides in soil by liquid-phase microextraction and gas chromatography-mass spectrometry. , 2004, Journal of chromatography. A.

[18]  S. Zorita,et al.  Development of a solid-phase extraction method for the determination of polychlorinated biphenyls in water. , 2004, Journal of chromatography. A.

[19]  C. Gourdon,et al.  Emulsification by ultrasound: drop size distribution and stability. , 1999, Ultrasonics sonochemistry.

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

[21]  C. Bondy,et al.  On the mechanism of emulsification by ultrasonic waves , 1935 .

[22]  R. Schwarzenbach,et al.  Phenyl- and butyltin analysis in small biological samples by cold methanolic digestion and GC/MS. , 2000, Analytical chemistry.

[23]  M. Díez,et al.  Organochlorine pesticide residues in bovine milk from Leon (Spain). , 1996, The Science of the total environment.

[24]  A. Kočan,et al.  Simple solid-phase extraction method for determination of polychlorinated biphenyls and selected organochlorine pesticides in human serum. , 2005, Journal of chromatography. A.

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

[26]  M. Jeannot,et al.  Solvent microextraction into a single drop. , 1996, Analytical chemistry.

[27]  David Julian McClements,et al.  Influence of flocculation on the ultrasonic properties of emulsions: theory , 1998 .

[28]  Hian Kee Lee,et al.  Liquid-Phase Microextraction in a Single Drop of Organic Solvent by Using a Conventional Microsyringe , 1997 .

[29]  H. Prosen,et al.  Solid-phase microextraction , 1999 .

[30]  Stanislav Emelianov,et al.  Acoustic radiation force and streaming induced by focused nonlinear ultrasound in a dissipative medium , 1996 .

[31]  C. Basheer,et al.  Dynamic hollow fiber-supported headspace liquid-phase microextraction. , 2005, Journal of chromatography. A.

[32]  F. Priego-Capote,et al.  Simultaneous ultrasound-assisted emulsification-extraction of polar and nonpolar compounds from solid plant samples. , 2007, Analytical chemistry.

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

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