Determination of 2-ethylhexyl 4-(dimethylamino) benzoate using membrane-assisted liquid-liquid extraction and gas chromatography-mass spectrometric detection

• Published in: Analytical and bioanalytical chemistry Vol. 394; no. 3; pp. 883 - 891
• Main Authors: March, J. G, Genestar, C, Simonet, B. M
• Format: Journal Article
• Language: English
• Published: Berlin/Heidelberg Berlin/Heidelberg : Springer-Verlag 01.06.2009; Springer Berlin Heidelberg; Springer
• Subjects: 4-Aminobenzoic Acid - urine; Analytical Chemistry; Benzoates; Biochemistry; Characterization and Evaluation of Materials; Chemical Fractionation - instrumentation; Chemical Fractionation - methods; Chemistry; Chemistry and Materials Science; Chromatographic methods and physical methods associated with chromatography; Ethanol - chemistry; Ethyl alcohol; Exact sciences and technology; Food Science; Gas chromatographic methods; Gas Chromatography-Mass Spectrometry; Humans; Hydrogen-Ion Concentration; Laboratory Medicine; Linearity; Membranes; Membranes, Artificial; Monitoring/Environmental Analysis; Original Paper; Other chromatographic methods; para-Aminobenzoates; Porosity; Potassium Chloride - chemistry; Potassium chlorides; Solvent extraction; Spectrometric and optical methods; Surface Properties; Time Factors; Urine; Wine - analysis; Wines; Urine; Wine; Micro-porous membrane liquid–liquid extraction; Gas chromatography-mass spectrometry; 2-Ethylhexyl 4-(dimethylamino) benzoate; Standard addition method; Porous membrane; Solvent extraction; Liquid liquid chromatography; Chemical enrichment; Sample preparation; Efficiency; Detection limit; Standard deviation; Quantitative analysis; Fluid mechanics; Micro-porous membrane liquid―liquid extraction; Ethanol; Liquid liquid extraction; Potassium chloride; Benzoate; Gas chromatography; Organic solvent; Sensitivity; Sample cell; Linearity; Gas liquid chromatography; Mass spectrometry; Microfluidics
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-009-2770-4

A flow-cell for micro-porous membrane liquid-liquid extraction with a sheet membrane was used to extract 2-ethylhexyl 4-(dimethylamino) benzoate (EDB) from urine of solar-cream users and spiked wine samples. The cell enabled the target analyte to be extracted from 7.9 mL of donor solution into 200 μL of acceptor solution (decane). After extraction, the acceptor solution was transferred to a micro-vial for GC-MS analysis without derivation. In this work, variables affecting the enrichment factor were also studied, such as organic solvent, extraction time, recirculation flow of the donor solution through the donor chamber, presence of potassium chloride and ethanol in the donor solution and pH. The method has been evaluated in terms of linearity, sensitivity, precision, limits of detection and quantification and extraction efficiency. Limits of quantification were 1 and 3 μg L⁻¹ EDB for urine and wine, respectively. Quantitative analysis has been carried out by applying the method of standard additions. Within- and between-day relative standard deviations were lower than 12% and 20%, respectively. EDB was found in the urine of users of cream containing EDB in the concentration interval 1.2-7.2 μg L⁻¹. Therefore, this provides evidence of EDB dermal absorption and subsequent excretion through the urinary tract. EDB was not found in the analysed wine samples.