Biomedical subjects

Maria Llompart

Publications and source records attributed to Maria Llompart.

24 records · Page 2Linked to original sources

PubMed2004

Development of a sensitive methodology for the analysis of chlorobenzenes in air by combination of solid-phase extraction and headspace solid-phase microextraction.

In this study, a combination of solid-phase extraction (SPE) and solid-phase microextraction (SPME) has been used to determine chlorobenzenes in air. Analytes were sampled by pumping a known volume of air through a porous polymer (Tenax TA). Then, the adsorbent was transferred into a glass vial and SPME was performed. The quantification was carried out using gas chromatography (GC)-electron-capture detection or GC-MS. Several SPME coatings (100 microm poly(dimethylsiloxane) (PDMS), 75 microm Carboxen (CAR)-PDMS, 65 microm PDMS-divinylbenzene (DVB), 65 microm PDMS-DVB and 85 microm polyacrylate (PA) were evaluated, obtaining the highest responses with Carbowax (CW)- PDMS for the most volatile chlorobenzenes, and with PDMS-DVB or CW-DVB fibers for the semivolatile compounds. To optimize some other factors that could affect the SPME step, a factorial design was used. Kinetic studies of the SPME process were also performed. Concerning the SPE step, breakthrough was studied, showing that 2.5 m3 of air could be processed without losses of the most volatile compounds. The performance of the method was evaluated. External calibration, which does not require the complete sampling process, demonstrated to be suitable, obtaining good linearity (R2 > 0.99) for all chlorobenzenes. Recovery studies were performed at two concentration levels (4 and 40 ng/m3), obtaining quantitative recoveries (>80%). Limits of detection at the sub ng/m3 were achieved for all the target compounds.

Air↗

PubMed2004

Study of the photoinduced degradation of polycyclic musk compounds by solid-phase microextraction and gas chromatography/mass spectrometry.

Polycyclic musks are widely used synthetic fragrances that have been identified during the last few years in biota samples and environmental matrices. Nevertheless, there is a lack of information concerning the photodegradation behavior of these compounds. In this work, the photoinduced degradation of six polycyclic musk compounds (Cashmeran, Celestolide, Phantolide, Galaxolide, Traseolide and Tonalide) was studied using a solid-phase microextraction (SPME) fiber as support. Musk fragrances were extracted from aqueous solutions using SPME fibers that were subsequently exposed to ultraviolet (UV) irradiation for different times. To study the degradation kinetics and to tentatively identify the photoproducts generated, gas chromatography coupled to ion trap mass spectrometry was used. Aqueous photodegradation studies were also performed. The on-fiber photodegradation approach avoids the need for further extraction processes and makes the identification of photoproducts easier, due to their higher concentration on the fibers. All musk compounds were easily photodegraded, suggesting that UV irradiation could work as a decontamination tool for these musks.

Journal Article↗

PubMed2003

Accelerated solvent extraction (ASE) of environmental organic compounds in soils using a modified supercritical fluid extractor.

Accelerated solvent extraction (ASE) has been applied to the quantitative extraction of a selected list of semi-volatiles, which include polycyclic aromatic hydrocarbons (PAHs), phenols, polychlorinated biphenyls (PCBs) and total petroleum hydrocarbons. Two conventional supercritical fluid extraction (SFE) systems, the Suprex Prep Master and SFE/50 systems have been modified to function as ASE systems. Using solvent instead of supercritical fluid, extraction in an enclosed system proceeded under high pressure and temperature. Parameters such as extraction temperature and effect of modifiers were investigated. Although limited by a 150 degrees C maximum oven temperature, effective extraction could be carried out in less than 25 min for all the compounds studied. The technique was applied to a variety of real matrices contaminated with hydrocarbons, PAHs and phenols. Validations of the technique were performed using standard reference materials. Recoveries for these matrices were good (>75%) and precision (R.S.D.) was generally less than 10%. Primarily a rapid field extraction technique, comparison with other rapid extraction such as sonication and microwave assisted extraction (MAP) were made. Recoveries were found to be comparable to MAP and superior to sonication. On the present ASE system, only sequential extraction can be carried out but given the rapid nature of the process, about 15 samples can be carried out in a working day.

Chemistry Techniques, Analytical↗

PubMed2002

Optimization of a derivatization-solid-phase microextraction method for the analysis of thirty phenolic pollutants in water samples.

Solid-phase microextraction (SPME) coupled to gas chromatography-mass spectrometry has been applied to the extraction of 30 phenol derivatives from water samples. Analytes were in situ acetylated and headspace solid-phase microextraction was performed. Different parameters affecting extraction efficiency were studied. Optimization of temperature, type of microextraction fiber and volume of sample has been done by means of a mixed-level categorical experimental design, which allows to study main effects and second order interactions. Five different fiber coatings were employed in this study; also, extraction temperature was studied at three levels. Both factors, fiber coating and extraction temperature, were important to achieve high sensitivity. Moreover, these parameters showed a significant interaction, which indicates the different kinetic behavior of the SPME process when different coatings are used. It was found that 75 microm carboxen-polydimethylsiloxane and 100 microm polydimethylsiloxane, yield the highest responses. The first one is specially appropriated for phenol, methylphenols and low chlorinated chlorophenols and the second one for highly chlorinated phenols. The two methods proposed in this study shown good linearity and precision. Practical applicability was demonstrated through the analysis of a real sewage water sample, contaminated with phenols.

Gas Chromatography-Mass Spectrometry↗

PubMed2002

Optimisation of a solid-phase microextraction method for synthetic musk compounds in water.

A solid-phase microextraction method (SPME) for determining trace levels of synthetic musk fragrances in residual waters has been developed. Six polycyclic musks (cashmeran, phantolide, celestolide, traseolide, galaxolide and tonalide), and a macrocyclic musk (ambrettolide) have been analysed. A detailed study of the different parameters affecting the extraction process is presented. The main important factors affecting the microextraction process have been studied and optimised by means of a categorical factorial design. Two extraction modes (direct SPME and headspace SPME) were tried at different extraction temperatures using four different fiber coatings [polydimethylsiloxane (PDMS), Carboxen (CAR)-PDMS, PDMS-divinylbenzene (DVB) and Carbowax (CW)-DVB]. An extraction temperature of 100 degrees C sampling the headspace over the sample using CAR-PDMS or PDMS-DVB as fiber coatings were found to be the experimental conditions that lead to a more effective extraction. The method proposed is very simple and yields high sensitivity, with detection limits in the low pg/ml, good linearity and repeatability for all the target compounds. The total analysis time, including extraction and GC analysis, was only 45 min. The optimised method performed well when it was applied to waste water from an urban treatment plant.

Fatty Acids, Monounsaturated↗

PubMedDate not supplied

Application of strategically designed sample composition to the rapid analytical screening of milk samples for polychlorinated biphenyls.

Strategically designed sample composition (SSC) is a new technique that decreases the number of analytical determinations needed in routine screening to as few as the number of original sample specimens while providing information that is specific to them. Although this new technique has been applied to environmental studies, this paper describes its first application to food safety studies. Contamination of milk samples with polychlorinated biphenyls (PCBs) was chosen as a case study to show the usefulness and potential of the SSC technique with a fast analytical procedure that involves saponification of the samples and solid-phase microextraction of the PCBs. A total of 20 sample specimens can be analyzed in 11 determinations with excellent predictions of the positive samples and the concentration levels of the contaminants. The robustness of the strategy was investigated and demonstrated.

Animals↗