18 resultados para HPLC-UV-PAD

em Consorci de Serveis Universitaris de Catalunya (CSUC), Spain


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Two concentration methods for fast and routine determination of caffeine (using HPLC-UV detection) in surface, and wastewater are evaluated. Both methods are based on solid-phase extraction (SPE) concentration with octadecyl silica sorbents. A common “offline” SPE procedure shows that quantitative recovery of caffeine is obtained with 2 mL of an elution mixture solvent methanol-water containing at least 60% methanol. The method detection limit is 0.1 μg L−1 when percolating 1 L samples through the cartridge. The development of an “online” SPE method based on a mini-SPE column, containing 100 mg of the same sorbent, directly connected to the HPLC system allows the method detection limit to be decreased to 10 ng L−1 with a sample volume of 100 mL. The “offline” SPE method is applied to the analysis of caffeine in wastewater samples, whereas the “on-line” method is used for analysis in natural waters from streams receiving significant water intakes from local wastewater treatment plants

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El programa experimental s’ha portat a terme dins el marc de les activitats del projecte TRUEFOOD, finançat per la UE per als anys 2007-2010. L’objectiu principal d’aquesta activitat ha estat l’avaluació dels continguts en àcid ascòrbic (vitamina C), polifenols totals, àcids fenòlics i flavonoides en mostres de tomàquet i enciam, produïts sota diferents condicions de camp (producció ecològica i convencional). Per aconseguir els resultats s’han utilitzat mètodes analítics basats en tècniques de cromatografia líquida d’alta eficàcia (HPLC) i d’ultra-alta eficàcia (UHPLC) acoblades a sistemes de detecció de diode array (DAD) i espectrometria de masses (MSn). Per a l’àcid ascòrbic, s’ha desenvolupat un mètode ràpid que ha permès la determinació d’aquest compost en diferents matrius vegetals amb el mínim pretractament de les mostres, utilitzant una fase estacionària HILIC (Fluorinated Stationary Phase). Els mètodes desenvolupats d’anàlisi de compostos fenòlics han permès realitzar les anàlisi de forma ràpida, a fi de processar el màxim nombre de mostres per a obtenir resultats representatius. S’ha realitzat una completa caracterització dels extractes de tomàquet i enciam, ampliant el coneixement descrit en la bibliografia sobre la seva composició fenòlica. En el cas de l’enciam, s’ha identificat quatre compostos fenòlics que mai abans han estat descrits i quantificats en aquesta hortalissa. La definició, amb precisió, dels continguts en vitamina C i compostos fenòlics en les mostres analitzades ha permès comparar els efectes de diferents tècniques de cultiu sobre les característiques nutricionals dels vegetals objecte de l’estudi. Els mètodes d’anàlisi desenvolupats i els resultats derivats del projecte seran publicats properament en revistes científiques de reconegut prestigi.

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Se prepararon partículas de nanocomposites basados en TiO2 y nanotubos de carbono multicapa platinizados para la obtención de combustibles solares. Se evaluó la actividad fotocatalítica del material en la producción de hidrógeno, en procesos de degradación de ácido fórmico, y en la obtención de hidrocarburos a partir de la reducción de CO2 en agua. Los nanocomposites fueron sintetizados por medio de la técnica sol-gel. Se estudió el efecto de la proporción y el diámetro de los nanotubos de carbono en la actividad del material bajo iluminación ultravioleta y visible. Se estudió el efecto de la adición de RuO2 (0,5% wt.) en la actividad bajo iluminación visible. Los materiales fueron caracterizados por ATR, XRD, BET, HRTEM y SEM. Se obtuvieron sólidos macroporosos, con contenido de fase anatasa superior al 99% y tamaño cristalino comprendido entre 15 y 21 nm. Los resultados cinéticos mostraron una producción óptima de hidrógeno para el composite TiO2/(5wt.%)MWCNT/Pt(60-80 nm), con eficiencia cuántica y eficiencia energética de 1,27% y 0,27%, respectivamente. En el caso de radiación visible, la producción de hidrógeno fue nula para los composites TiO2/MWCNT/Pt, mientras que para el sistema RuO2/TiO2/MWCNT/Pt se observó que la adicción de MWCNT inhibía la actividad fotocatalítica del composite RuO2/TiO2 en la región del visible. Por otra parte, en los ensayos de reducción de CO2 no se detectó ningún producto de reacción.

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The purpose of this work is determine the extent of closure between measurements and models of UV irradiances at diverse sites using state of the art instruments, models, and the best available data as inputs to the models. These include information about aerosol optical depth (unfortunately not extending down as far into the UVB region as desirable because such information is not generally available), ozone column amounts, as well as vertical profiles of temperature. We concentrate on clear-sky irradiances, and report the results in terms of UV Index (UVI)

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To perform a climatic analysis of the annual UV index (UVI) variations in Catalonia, Spain (northeast of the Iberian Peninsula), a new simple parameterization scheme is presented based on a multilayer radiative transfer model. The parameterization performs fast UVI calculations for a wide range of cloudless and snow-free situations and can be applied anywhere. The following parameters are considered: solar zenith angle, total ozone column, altitude, aerosol optical depth, and single-scattering albedo. A sensitivity analysis is presented to justify this choice with special attention to aerosol information. Comparisons with the base model show good agreement, most of all for the most common cases, giving an absolute error within 0.2 in the UVI for a wide range of cases considered. Two tests are done to show the performance of the parameterization against UVI measurements. One uses data from a high-quality spectroradiometer from Lauder, New Zealand [45.04°S, 169.684°E, 370 m above mean sea level (MSL)], where there is a low presence of aerosols. The other uses data from a Robertson–Berger-type meter from Girona, Spain (41.97°N, 2.82°E, 100 m MSL), where there is more aerosol load and where it has been possible to study the effect of aerosol information on the model versus measurement comparison. The parameterization is applied to a climatic analysis of the annual UVI variation in Catalonia, showing the contributions of solar zenith angle, ozone, and aerosols. High-resolution seasonal maps of typical UV index values in Catalonia are presented

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The interest in solar ultraviolet (UV) radiation from the scientific community and the general population has risen significantly in recent years because of the link between increased UV levels at the Earth's surface and depletion of ozone in the stratosphere. As a consequence of recent research, UV radiation climatologies have been developed, and effects of some atmospheric constituents (such as ozone or aerosols) have been studied broadly. Correspondingly, there are well-established relationships between, for example, total ozone column and UV radiation levels at the Earth's surface. Effects of clouds, however, are not so well described, given the intrinsic difficulties in properly describing cloud characteristics. Nevertheless, the effect of clouds cannot be neglected, and the variability that clouds induce on UV radiation is particularly significant when short timescales are involved. In this review we show, summarize, and compare several works that deal with the effect of clouds on UV radiation. Specifically, works reviewed here approach the issue from the empirical point of view: Some relationship between measured UV radiation in cloudy conditions and cloud-related information is given in each work. Basically, there are two groups of methods: techniques that are based on observations of cloudiness (either from human observers or by using devices such as sky cameras) and techniques that use measurements of broadband solar radiation as a surrogate for cloud observations. Some techniques combine both types of information. Comparison of results from different works is addressed through using the cloud modification factor (CMF) defined as the ratio between measured UV radiation in a cloudy sky and calculated radiation for a cloudless sky. Typical CMF values for overcast skies range from 0.3 to 0.7, depending both on cloud type and characteristics. Despite this large dispersion of values corresponding to the same cloud cover, it is clear that the cloud effect on UV radiation is 15–45% lower than the cloud effect on total solar radiation. The cloud effect is usually a reducing effect, but a significant number of works report an enhancement effect (that is increased UV radiation levels at the surface) due to the presence of clouds. The review concludes with some recommendations for future studies aimed to further analyze the cloud effects on UV radiation

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This article summarizes the basic principles of photoelectron spectroscopy for surface analysis, with examples of applications in material science that illustrate the capabilities of the related techniques.

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Lasers are essential tools for cell isolation and monolithic interconnection in thin-film-silicon photovoltaic technologies. Laser ablation of transparent conductive oxides (TCOs), amorphous silicon structures and back contact removal are standard processes in industry for monolithic device interconnection. However, material ablation with minimum debris and small heat affected zone is one of the main difficulty is to achieve, to reduce costs and to improve device efficiency. In this paper we present recent results in laser ablation of photovoltaic materials using excimer and UV wavelengths of diode-pumped solid-state (DPSS) laser sources. We discuss results concerning UV ablation of different TCO and thin-film silicon (a-Si:H and nc-Si:H), focussing our study on ablation threshold measurements and process-quality assessment using advanced optical microscopy techniques. In that way we show the advantages of using UV wavelengths for minimizing the characteristic material thermal affection of laser irradiation in the ns regime at higher wavelengths. Additionally we include preliminary results of selective ablation of film on film structures irradiating from the film side (direct writing configuration) including the problem of selective ablation of ZnO films on a-Si:H layers. In that way we demonstrate the potential use of UV wavelengths of fully commercial laser sources as an alternative to standard backscribing process in device fabrication.

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A mathematical model of the voltage drop which arises in on-chip power distribution networks is used to compare the maximum voltage drop in the case of different geometric arrangements of the pads supplying power to the chip. These include the square or Manhattan power pad arrangement, which currently predominates, as well as equilateral triangular and hexagonal arrangements. In agreement with the findings in the literature and with physical and SPICE models, the equilateral triangular power pad arrangement is found to minimize the maximum voltage drop. This headline finding is a consequence of relatively simple formulas for the voltage drop, with explicit error bounds, which are established using complex analysis techniques, and elliptic functions in particular.

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ZnO nanorods grown by both high temperature vapour phase transport and low temperature chemical bath deposition are very promising sources for UV third harmonic generation. Material grown by both methods show comparable efficiencies, in both cases an order of magnitude higher than surface third harmonic generation at the quartz-air interface of a bare quartz substrate. This result is in stark contrast to the linear optical properties of ZnO nanorods grown by these two methods, which show vastly different PL efficiencies. The third harmonic generated signal is analysed using intensity dependent measurements and interferometric frequency resolved optical gating, allowing extraction of the laser pulse parameters. The comparable levels of efficiency of ZnO grown by these very different methods as sources for third harmonic UV generation provides a broad suite of possible growth methods to suit various substrates, coverage and scalability requirements. Potential application areas range from interferometric frequency resolved optical gating characterization of few cycle fs pulses to single cell UV irradiation for biophysical studies.

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In this work methods for the multiresidue determination of the series of quinolones include in the European regulation in food of animal origin are de veloped and validated in line with Commission Decision 2002/657/EC in terms of linearity, decision limit, capability detection, precision and stability. Mult iresidue methods were established to allow the determination of quinolones covered by EU legislation in 2377/90/EC in muscle of chicken, turkey, pig and cow, plasma of cow and pig, liver of pig and milk of cow. First an extraction step was optimized and a SPE step was applied to clean!up and preconcentrate quinolones prior to their separation by CE or LC and determination by CE!UV, LC!UV, LC!Fl, LC!MS with different ion sources (ESI ,ApCI) and different mass analyser (Q, ToF) and LC!E SI!QqQ tandem mass spectrometry. The limits of quantification obtained are always lower than Maxim um Residue Limit (MRL) established by EU for quinolones in animal products and they can be applied to the control of quinolones in foodstuffs of animal origin . Finally the proposed methods were applied to determine quinolones in samples of turkey and pig muscle, pig plasma and milk of cow. Excellent quality parameters and reduced time of analysis were obtained when LC!ESI!MS/MS is used, although the others techniques presented too satisfactory results.

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Per poder desenvolupar un producte farmacèutic és necessari establir un mètode d’anàlisis que permeti determinar i quantificar totes aquelles substàncies que conté, ja sigui referent als principis actius; a les impureses i productes de degradació, conservants, antioxidants,... Grans entitats com la ICH remarquen la importància de validar els mètodes analítics ja que és la via per demostrar que aquell producte compleix les garanties de qualitat prèviament establertes. Així doncs, l’objectiu d’aquest Treball Final de Grau és poder desenvolupar i validar dos mètodes analítics per a la determinació d’aminoàcids i carbohidrats respectivament, d’un producte farmacèutic per cromatografia líquida (HPLC). Per tal de poder concloure que aquell mètode és adequat per la determinació per la qual ha estat desenvolupat, és necessari obtenir resultats que compleixin els criteris d’acceptació corresponents als paràmetres que han de ser avaluats en una validació analítica. Aquests paràmetres són: la precisió, la selectivitat, l’exactitud i la linealitat i el rang. Els resultats d’aquest projecte han demostrat que els dos mètodes desenvolupats són adequats per a la determinació de tres dels principis actius (aminoàcid 1, aminoàcid 2 i carbohidrat 1) que conté el producte farmacèutic d’ús veterinari analitzat; i poden ser validats ja que compleixen els criteris d’acceptació dels paràmetres avaluats que proposa la ICH. El mètode per la determinació de carbohidrats no és vàlid per el carbohidrat 2, ja que durant el desenvolupament es va detectar que una bona part d’aquest passava a carbohidrat 1 (desplaçament de l’equilibri ceto-enòlic que hi ha entre el carbohidrat 1 i el carbohidrat 2 a pHs alts). És per aquest motiu, que es pot concloure que aquest mètode no és vàlid i es recomana seguir investigant per a poder desenvolupar un mètode analític adient.

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Objectives: To determine the efficacy of the pediculate flap with the buccal fat pad in the sealing of orosinusal communications, describe the surgical technique used, and report the main complications. Patients and method: A retrospective study was made of 8 patients seen in the Service of Oral Surgery of the University of Barcelona Dental Clinic (Spain) for the treatment of orosinusal communications between the years 2007 and 2009. In all cases a pediculate flap with the buccal fat pad was used to solve the problem. Results: All of the orosinusal communications were successfully resolved with this technique. The immediate postoperative complications were pain (37.5%), inflammation (37.5%), edema (32.5%), trismus (37.5%), halitosis (14.3%), suppuration (12.5%) and rhinorrhea (12.5%). Conclusions: The use of Bichat"s buccal fat pad is not regarded as the technique of choice for sealing small to medium sized orosinusal communications. However, in the case of large communications, it is a good option, and the results obtained are optimum.

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A mathematical model of the voltage drop which arises in on-chip power distribution networks is used to compare the maximum voltage drop in the case of different geometric arrangements of the pads supplying power to the chip. These include the square or Manhattan power pad arrangement, which currently predominates, as well as equilateral triangular and hexagonal arrangements. In agreement with the findings in the literature and with physical and SPICE models, the equilateral triangular power pad arrangement is found to minimize the maximum voltage drop. This headline finding is a consequence of relatively simple formulas for the voltage drop, with explicit error bounds, which are established using complex analysis techniques, and elliptic functions in particular.