Lurdes I.B. Silva

Optical fiber biosensor coupled to chromatographic separation for screening of dopamine, norepinephrine and epinephrine in human urine and plasma

An optical fiber biosensor has been developed for the determination of catecholamines (dopamine, norepinephrine and epinephrine) based on the recognition capacity of the enzyme laccase. In this study, a glass tube constituted by a fused silica fiber coated with a film of polystyrene/divinylbenzene resin (PS/DVB) was used for catecholamines separation. Firstly, the analyzer was tested for calibration and its analytical performance for catecholamines detection was compared with a classical analytical method, namely high performance liquid chromatography-electrochemical detector (HPLC-ED). The developed analytical device shows a high potential for catecholamines quantification with a detection limit of 2.1, 2.6 and 3.4 pg mL(-1) for dopamine, norepinephrine and epinephrine, respectively. The analytical sensitivity, inferred from the slope of the calibration curves established for a range of concentrations between 5 and 125 pg mL(-1), was found to be 0.344, 0.252 and 0.140 dB/pg mL(-1) for dopamine, norepinephrine and epinephrine, respectively. Furthermore, catecholamines speciation with the PS/DVB fiber was completely achieved in 3 min. The analytical performance of the reported sensor was also evaluated and found adequate for catecholamines determination in human urine and plasma samples.

High performance liquid chromatography coupled to an optical fiber detector coated with laccase for screening catecholamines in plasma and urine

An analytical method based on separation by high performance liquid chromatography (HPLC) and detection by optical fiber (OF) coated with an enzyme (laccase), has been developed for separation and quantification of catecholamines, namely epinephrine, dopamine and norepinephrine. The application of OF as a detector in this analytical system relies on the variation of the reflected optical power detected when the catecholamines eluted from the HPLC column act as the substrate of the laccase immobilized on a tip of a single-mode OF. The developed method shows a high linearity in a range between 5 and 125 pg/mL and detection limits of 3.5, 2.9 and 3.3 pg/mL for epinephrine, dopamine and norepinephrine, respectively. The analytical performance of the proposed method was compared with a classical analytical method, namely high performance liquid chromatography-electrochemical detector (HPLC-ED) regarding catecholamines detection, showing great analytical advantages such as low cost of equipment. Additionally, the proposed method was applied to catecholamines determination in actual samples of plasma and human urine.

Breath analysis by optical fiber sensor for the determination of exhaled organic compounds with a view to diagnostics.

Breath analysis constitutes a promising tool in clinical and analytical fields due to its high potential for non-invasive diagnostics of metabolic disorders and monitoring of disease status. An optical fiber (OF) sensor has been developed for determination of volatile organic compounds (ethane, pentane, heptane, octane, decane, benzene, toluene and styrene) in human breath for clinical diagnosis. The analytical system developed showed a high performance for breath analysis, inferred for the analytical signal intensity and stability, linear range, and detection limits ranging from 0.8 pmol L(-1), for heptane, and to 9.5 pmol L(-1), for decane. The OF sensor also showed advantageous features of near real-time response and low instrumentation costs, besides showing an analytical performance equivalent to the breath analysis by gas chromatography-mass spectrometry (GC-MS), used as the reference method.

Remote optical fibre microsensor for monitoring BTEX in confined industrial atmospheres.

A portable optical fibre sensor has been developed for remote monitoring of benzene, toluene, ethylbenzene, p-xylene, m-xylene and o-xylene (BTEX). Firstly, the analyser was tested for calibration and its analytical performance for BTEX monitoring compared with a more classical analytical method, namely gas chromatography coupled to a flame ionization detector (GC-FID). The developed remote sensor shows several analytical advantages such as, high analytical sensitivity and accuracy, good linearity and stability of the analytical signal and short analytical time. Secondly, the optical fibre based sensor was applied to air monitoring for detection and quantification of BTEX in a confined industrial environment. The analytical signal measurement was performed by wireless at 20 m of distance from the local of analysis. Besides, the reported sensor showed a high degree of portability, compact design and high analytical performance for remote BTEX monitoring, in situ and in real-time.

Comparison of a gas chromatography-optical fibre (GC-OF) detector with a gas chromatography-flame ionization detector (GC-FID) for determination of alcoholic compounds in industrial atmospheres

An analytical methodology based on an optical fibre detector coupled to gas chromatograph has been developed for the speciation of some volatile alcoholic compounds. This methodology combines the separation capability of gas chromatography with an optical fibre detector made of an optical fibre sensitized with a thin polymeric film of poly[methyl(3,3,3-trifluoropropyl)siloxane] (PMTFPS). The response of the detector has been characterized at 650 nm for nine different alcohols (allyl alcohol, n-propyl alcohol, sec-butyl alcohol, isobutyl alcohol, n-butyl alcohol, isoamyl alcohol, methyl isobutyl carbinol, cyclohexanol and diacetone alcohol). An alternative method based on gas chromatography-flame ionization detector (GC-FID) was also used in order to evaluated the performance and compare the analytical results with the proposed method. The time of analysis, the analytical error and the analytical performance were similar for both methods. However, the analytical apparatus based on the GC-OF detector is much less expensive than the GC-FID and show high accuracy and suitability for actual monitoring on indoor atmospheres.

Polymeric nanofilm-coated optical fibre sensor for speciation of aromatic compounds

An optical fibre sensor has been shown to be suitable for monitoring of benzene, toluene and o-xylene (BTX) with both high selectivity and sensitivity. The sensing principle underlying this experimental device is based on the changes of the reflected optical power when BTX vapours are present in the analytical tube containing an optical fibre coated with a thin film of poly[methyl(3, 3, 3-trifluoropropyl)siloxane]. The interaction of organic vapour with the sensitive surface promotes a variation of the light power, proportional to the amount of adsorbed BTX vapour. A set of experiments concerning different operational conditions was performed in order to promote a higher analytical performance and the newly developed BTX sensor showed higher sensitivity and shorter analytical time than a method based on gas chromatography–flame ionisation detector. Furthermore, the proposed sensor also provides the basis for an inexpensive analytical technique with adequate specificity for measurements of BTX at trace levels with appropriate reversibility, repeatability, and reproducibility. Finally, the analytical performance of the developed sensor was also evaluated and found adequate for industrial air samples.

Assessment of fatty acid as a differentiator of usages of urban soils

The determination of fatty acids (FA) has been extensively used as a sensitive and reproducible parameter for characterizing the soil microorganism communities and to detect various environmental stresses. The aim of this study was to assess the variability of FA in urban soils, in an attempt to use it as a differentiator of urban soil usage. FA were extracted from soils of five different usages (ornamental gardens, ornamental gardens/roadsides, roadsides, parks and urban agricultural areas) in three Portuguese cities and FA concentration was determined by gas chromatography coupled to mass spectrometry (GC-MS). A total of fifteen FA have been detected and the concentration of each FA, in general, decreased in the following order: Lisbon>Estarreja>Viseu, for all the usages of urban soil. According to soil microbial indicators, the concentration of Gram-negative bacteria was lower than the concentration of Gram-positive bacteria, which together were, in turn, higher than the concentration of fungi for all the usages of urban soil and city. This study assessed the FA profiles of urban soils, which differ as a function of soil usage. The FA profile also is at the source of the inference that stress in soil microorganism communities results from the different urban environment in each city.

Evaluation of tertiary treatment by fungi, enzymatic and photo-Fenton oxidation on the removal of phenols from a kraft pulp mill effluent: a comparative study.

Pulp and paper mills generate pollutants associated to their effluents depending upon the type of process, type of the wood materials, process technology applied, management practices, internal recirculation of the effluent for recovery, the amount of water used in the industrial process and type of secondary treatment. This study is the first that reports a simultaneous evaluation of the effects of tertiary treatments by fungi (Rhizopus oryzae and Pleurotus sajor caju), by enzyme (laccase) and by an oxidation process (photo-Fenton) on individual phenols (vanillin, guaiacol, phloroglucinol, vanillic acid and syringic acid) of a Eucalyptus globulus bleached kraft pulp and paper mill final effluent after secondary treatment (BKPME). The tertiary treatments were applied on BKPME samples and in BKPME samples supplemented with extra concentration of each phenol. Tertiary treatments by Rhizopus oryzae and photo-Fenton oxidation were able of complete removal (100%) of phenols on BKPME samples whereas P. sajor caju and laccase were able of 60–85% removal. On BKPME samples with added concentration of each phenol, photo-Fenton was the only treatment capable of total phenols removal (100%), which suggests a great potential for its application.

Gas chromatography - optical fiber detector for assessment of fatty acids in urban soils.

Fatty acids have been used as biomarkers of the microbial community composition of soils and they are usually separated and quantified by gas-chromatography coupled to a flame ionization detector (GC-FID). The aim of this study was to develop, validate and apply a methodology based on gas chromatography coupled to optical fiber detection (GC-OF) for screening five fatty acids used as indicators of fungal and bacterial communities in urban soils. The performance of the GC-OF methodology (optical fiber detector at 1,550 nm) was evaluated by comparison with the GC-FID methodology and it was found that they were comparable in terms of linear range, detection limit and analytical errors. Besides these similar analytical characteristics, the GC-OF is much cheaper than the GC-FID methodology. Different concentrations were determined for each fatty acid indicator which in turn varied significantly between the soil samples analyzed from Lisbon ornamental gardens. Additionally, the GC-OF showed a great potential as alternative for determination of eleven or more fatty acids in urban soils.

A fluorescence-based optical fiber analyzer for catecholamine determination

An optical fibre (OF) analyzer for measuring catecholamines (dopamine, norepinephrine and epinephrine) in biological samples with induced fluorescence was developed. The analytical set-up included a chromatographic column for catecholamine separation and a fluorescence-based OF detection (FOF-analyzer). The detection limit of the FOF-analyser was found to be less than 0.9 pg mL−1. The proposed methodology showed an adequate analytical performance for the determination of the catecholamines in actual samples of human urine. The analytical performance of the FOF-analyzer for catecholamine determination was investigated against the high performance liquid chromatography-electrochemical detection (HPLC-ED) method. The FOF-analyzer showed lower detection limits and larger linear ranges for determination of dopamine (DA), norepinephrine (NE) and epinephrine (E) in comparison with HPLC-ED and other methodologies such as HPLC-fluorescence. These advantages combined with the compact design, small-scale instrumentation, and effective cost of analysis make this system an interesting alternative to the existing methodologies for the determination of catecholamines in clinical samples.