A simple, inexpensive, and environmentally friendly method based on ultrasound-assisted emulsification microextraction followed by solidification of floating organic drop and high-performance liquid chromatography coupled to diode array detection was developed for the simultaneous determination of 18 potentially allergenic fragrance substances. Several parameters affecting the microextraction process were investigated in detail by the "one-variable-at-a-time" approach. Optimal conditions were the following: 50 μL of 2-dodecanol as extraction solvent, 10 mL of sample containing 150 g/L of salt, and 5 min of sonication at 35°C.
View Article and Find Full Text PDFIn this work, a simple and reliable micellar electrokinetic chromatography method for the separation and quantification of 14 preservatives, including isothiazolinones, and two benzophenone-type UV filters in household, cosmetic and personal care products was developed. The selected priority compounds are widely used as ingredients in many personal care products, and are included in the European Regulation concerning cosmetic products. The electrophoretic separation parameters were optimized by means of a modified chromatographic response function in combination with an experimental design, namely a central composite design.
View Article and Find Full Text PDFA nonaqueous micellar electrokinetic chromatography method was developed for determination of Tonalide®, Galaxolide®, and Traseolide® polycyclic musks (PCMs). These compounds are widely used as fragrance ingredients in cosmetics. The method was optimized by using a three variable Box-Behnken experimental design and response surface methodology.
View Article and Find Full Text PDFThe aim of this study was to measure of serum levels of p,p'-dichlorodiphenyl trichloroethane (p,p'-DDT), p,p'-dichlorodiphenyl dichlorethylene (p,p'-DDE), beta-hexachlorocyclohexane (beta-HCH), and hexachlorobenzene (HCB) in healthy adults in Spain. Furthermore, we also analyzed these levels according to dietary, other lifestyle factors and anthropometric characteristics. We measured the concentrations of such organochlorine pesticides (OCPs) in serum samples collected during 1992-1996 from 953 subjects aged 35-64 years, they were residents of five Spanish regions, they were randomly selected from the European Prospective Investigation into Cancer and Nutrition (EPIC) cohort.
View Article and Find Full Text PDFA gel permeation chromatographic (GPC) clean-up based method was developed for determination of selected organochlorine pesticides and polychlorinated biphenyls in human serum. The method permits automation of the sample extract clean-up stage and is designed to work with small amounts of sample. Different working variables were studied in its development, including injection volume, flow rate, and fat amount as the most representative coextract.
View Article and Find Full Text PDFThe European Water Framework Directive (WFD) establishes a framework for the protection and improvement of estuarine (transitional) and coastal waters, attempting to achieve good water status by 2015; this includes, within the assessment, biological and chemical elements. The European Commission has proposed a list of priority dangerous substances (including metals such as Cd, Hg, Ni and Pb), with the corresponding list of environmental quality standards (EQS), to assess chemical status, but only for waters. In this contribution, a long-term (1995-2007) dataset of transitional and coastal water and sediment trace elements concentrations, from the Basque Country (northern Spain), has been used to investigate the response of these systems to water treatment programmes.
View Article and Find Full Text PDFBackground: Polychlorinated biphenyls (PCBs) are persistent compounds that may pose an environmental hazard to humans, food being the main source of exposure for the general population.
Objective: To measure the serum concentrations of the main PCBs in subjects from the general population in Spain, and to assess potential determinants of such concentrations.
Methods: Serum was obtained from blood samples of 953 subjects aged 35-64 years, residents in five Spanish regions (three from the North and two from the South), randomly selected from the EPIC-Spain cohort.
Two simple methods using headspace solid-phase microextraction (HS-SPME) coupled to a gas chromatograph with a flame ionization detector were compared for the determination of polycyclic aromatic hydrocarbons (PAH) in soils. These compounds were included in the US Environmental Protection Agency's Priority Pollutants list. Direct hot water HS-SPME extraction and sonication organic extraction followed by HS-SPME were optimized using experimental designs.
View Article and Find Full Text PDFJ Chromatogr B Analyt Technol Biomed Life Sci
June 2007
An improved method for the determination of selected organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in human serum was developed. The method requires low volume of serum (500 microl) and 48-96 samples per day can be prepared by one analyst without special automatic equipment. Initial extraction was performed using 96-well solid-phase extraction disk plates and was followed by a clean-up with silica gel/sulfuric acid.
View Article and Find Full Text PDFJ Chromatogr B Analyt Technol Biomed Life Sci
February 2007
A simple procedure for the determination of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in human serum using headspace solid-phase microextraction (HS-SPME) was developed. The analysis was carried out by gas chromatography (GC) equipped with electron capture detector (ECD). A 2(7-4) Plackett-Burman reduced factorial design for screening and a central composite design for optimizing the significant variables were applied.
View Article and Find Full Text PDFA simple procedure for the determination of methyl tert-butyl ether (MTBE), ethyl tert-butyl ether (ETBE), ethyl butyl ether (EBE), tert-amyl methyl ether (TAME), benzene, toluene, ethylbenzene, and xylenes (BTEX) in water using headspace (HS) solid-phase microextraction (HS-SPME) was developed. The analysis was carried out by gas chromatography (GC) equipped with flame ionization detector (FID) and 100% dimethylpolysiloxane fused capillary column. A 2 Plackett-Burman design for screening and a central composite design (CCD) for optimizing the significant variables were applied.
View Article and Find Full Text PDFA procedure for determination of methyl tert.-butyl ether (MTBE) in water by headspace solid-phase microextraction (HS-SPME) has been developed. The analysis was carried out by gas chromatography with flame ionization detection.
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