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Hollow fibre liquid phase microextraction of parabens

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EN
A hollow fibre liquid phase microextraction for gas chromatographic determination of some p-hydroxybenzoic acid esters has been developed. Chlorobenzene containing tetradecane as internal standard was used for the extraction. Optimized extraction was carried out at room temperature for 40 min in the presence of 0.4 g mL−1 NaCl in the sample solution. Calibration was linear up to 30 mg L−1. Correlation coefficients were 0.996–0.998. Enrichment factors were 21, 95 and 154, and detection limits were 0.20, 0.03 and 0.01 μg mL−1 for methylparaben, ethylparaben and propylparaben, respectively. Reproducibility was acceptable with relative standard deviations up to 11.7%. The technique was tested for water and urine analysis. [...]
EN
The analytical microextraction methods of gas chromatography coupled with flame ionisation detector (GC-FID) for determination of selected essential oils in herbs were proposed. Two microextraction methods for the isolation of essential oils from plants such as Lavandula spica L., Melissa officinalis L., Mentha piperita L. and Salvia officinalis L. were used. The methods of solid-phase and single-drop microextractions, were optimised and compared. The obtained LOD values for all studied essential oils were found to be within 2.5–20.5 μg for SDME and 57.0–139.8 μg for SPME method per 100 g of dried sample leaves. The appropriate LOQ values were then 8.4–68.4 μg for SDME and 189.8–466.1 μg for SPME of target analytes per 100 g of dried sample leaves. [...]
EN
Seven alkyl methylphosphonic acids, products of hydrolytic degradation of organophosphorus chemical warfare agents, were obtained with a high purity (mostly above 98%), with the aim of being applyed as future certified reference materials. Ethyl (EMPA), isopropyl (IMPA), pinacolyl (PMPA), butyl (BUMPA), isobutyl (IBUMPA), cyclohexyl (CHMPA) and 2-ethylhexyl (EHMPA) monoesters of MPA were synthesized and characterized by MS EI, FTIR and NMR (1H, 13C, 31P), TLC, as well as GC and GC-MS after derivatization. The conditions for a direct quantitative GC FID analysis on CP-FFAP CB column of non-derivatized alkyl methylphosphonic acids were developed. This is the first successful attempt of a directed GC analysis of free alkyl phosphonic acids. Their chemical purity was determined and limit of quantification (LOQ) values for some of them were evaluated for the GC-FID method.
EN
The purpose of this study was to evaluate the decay of squalene and the formation of trans fatty acids (TFAs) in the amaranth oil extracted with hexane with and without heat. Oils were analyzed by determining their chemical values, and the fatty acids were identified and quantified by using Fourier-transform infrared (FTIR) spectroscopy, in the mid-region of 400–4000 cm−1, and gas chromatography. The FTIR analysis shows that two oil extracts (with and without heat) present a well-defined peak at 968 cm−1, which represents the trans double bonds. The quantified TFAs are [...]
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