Biomedical subjects

Guillermo Quintás

Publications and source records attributed to Guillermo Quintás.

6 recordsLinked to original sources

PubMed2006

Determination of peroxide-based explosives using liquid chromatography with on-line infrared detection.

A nondestructive analytical method for peroxide-based explosives determination in solid samples is described. Reversed-phase high-performance liquid chromatography in combination with on-line Fourier transform infrared (FT-IR) detection is used for the analysis of triacetonetriperoxide (TATP) and hexamethylenetriperoxide diamine (HMTD). In contrast to other liquid chromatographic methods with optical detection, no derivatization or decomposition of the peroxides is required. The peroxides are identified and quantified via their characteristic absorption spectra in the mid-infrared range of the electromagnetic spectrum. The detection limit of 0.5 mmol L-1 for HMTD and 1 mmol L-1 for TATP allows the identification of the explosives in complex matrixes.

Journal Article↗

PubMed2006

On-line monitoring of pH junctions in capillary electrophoresis using Fourier transform infrared spectrometry.

Fourier transform mid-infrared spectroscopic detection is proposed as an on-line detection technique for the study of on-line preconcentration processes in capillary electrophoresis (CE). The molecule-specific information contained in mid-IR spectra can be used to directly determine the chemical compositions of individual zones and their boundaries. This paper reports on pH junctions employed in myoglobin analysis. On-line mid-IR detection allowed the shape of the sample peak to be monitored as well as the chemical compositions of the surrounding zones. From this information it was possible to obtain detailed insights into the actual chemical compositions of the individual zones governing the efficiency of the preconcentration technique applied. The principle of measurement outlined here can therefore also be regarded as a promising one for investigating other on-line preconcentration techniques, like stacking, sweeping, and pH junction-sweeping among others.

Journal Article↗

PubMed2006

Automated sample preparation and analysis using a sequential-injection-capillary electrophoresis (SI-CE) interface.

A fully automated sequential-injection-capillary electrophoresis (SI-CE) system was developed using commercially available components as the syringe pump, the selection and injection valves and the high voltage power supply. The interface connecting the SI with the CE unit consisted of two T-pieces, where the capillary was inserted in one T-piece and a Pt electrode in the other (grounded) T-piece. By pressurising the whole system using a syringe pump, hydrodynamic injection was feasible. For characterisation, the system was applied to a mixture of adenosine and adenosine monophosphate at different concentrations. The calibration curve obtained gave a detection limit of 0.5 microg g(-1) (correlation coefficient of 0.997). The reproducibility of the injection was also assessed, resulting in a RSD value (5 injections) of 5.4%. The total time of analysis, from injection, conditioning and separation to cleaning the capillary again was 15 minutes. In another application, employing the full power of the automated SIA-CE system, myoglobin was mixed directly using the flow system with different concentrations of sodium dodecyl sulfate (SDS), a known denaturing agent. The different conformations obtained in this way were analysed with the CE system and a distinct shift in migration time and decreasing of the native peak of myoglobin (Mb) could be observed. The protein samples prepared were also analysed with off-line infrared spectroscopy (IR), confirming these results.

Journal Article↗

PubMed2005

FTIR approaches for diuron determination in commercial pesticide formulations.

Two strategies have been developed for Diuron determination by FTIR spectrometry, an off-line extraction and stopped-flow determination and a fully mechanized procedure, based on the on-line extraction of Diuron and FIA-FTIR measurement of the extracts. The aforementioned procedures have been compared with a reference chromatographic method. The off-line FTIR spectra were obtained at a nominal resolution of 4 cm(-1) from 4000 to 900 cm(-1) by accumulating 25 scans. Diuron was determined using peak height measurements at 1582 cm(-1) corrected using a baseline defined between 1562 and 1614 cm(-1). The waste generation of the off-line procedure was 3.4 mL chloroform for each sample, and the method provided a LOD of 40 microg g(-1), corresponding to 0.8% (w/w) Diuron in the original sample. The fully mechanized FIA method provided a LOD of 35 microg g(-1), which corresponds to 0.7% (w/w) in the solid sample and a maximum sampling frequency of the whole procedure of 30 h(-1), with a waste generation of 9.3 mL per sample, taking into account the volume of CHCl(3) required for sample dissolution and that need as a carrier. All those methods consume less organic solvent than a HPLC method, which involves the use of 39 mL of acetonitrile per sample and a sampling frequency of 12 h(-1).

Chromatography, High Pressure Liquid↗

PubMed2002

Determination of caffeine in tea samples by Fourier transform infrared spectrometry.

A sustainable and environmentally friendly procedure has been developed for the FTIR determination of caffeine in tea leaf samples. The method is based on the extraction with ammonia and CHCl3 and direct determination of caffeine on the chloroform extracts using peak height absorbance measurements at 1658.5 cm(-1) and external calibration. The method provides a sensitivity of 0.2142 absorbance units mg(-1) mL and a limit of detection of 1 mg L(-1), corresponding to 0.002% m/m caffeine in tea leaves. As compared with a reference procedure, based on UV absorbance measurement at 276 nm after low pressure column chromatography, the developed procedure reduces the consume of CHCl3 by a factor of 10, that of NH4OH by a factor of 20 and avoids the use of diethyl ether and Celite. The time required to do the analysis of a sample is 15 minutes as compared with the 6 hours for the reference one.

Caffeine↗

PubMedDate not supplied

Determination of pirimicarb and endosulfan in commercial pesticide formulations by Fourier transform infrared spectrometry.

A routine method based on Fourier transform infrared spectrometry was developed for the simultaneous determination of pirimicarb and endosulfan in commercially available pesticide formulations. The method is based on peak area absorbance measurements between 1362 and 1352 cm(-1), corrected with a baseline fixed at 1338 cm(-1), for pirimicarb and peak area absorbance measurements between 919 and 909 cm(-1) with a baseline fixed at 931 cm(-1) for endosulfan; chloroform solutions for analysis were obtained by direct dilution of emulsifiable concentrates or by solvent extraction from solid samples. Various extraction conditions and appropriate band selection were investigated, and interference studies were performed. Under the experimental conditions selected, limits of detection of 13 microg/g for pirimicarb and 150 microg/g for endosulfan were obtained that correspond to 0.13 and 1.6% (w/w), respectively, in commercial samples. Results from analyses of commercial samples by the developed method compared well with those obtained by a liquid chromatography reference method.

Calibration↗