Real-Time Measurement of Refractive Index Using 3D-Printed Optofluidic Fiber Sensor.

This work describes a 3D-printed optofluidic fiber sensor to measure refractive index in real time, combining a microfluidic system with an optical fiber extrinsic Fabry-Perot interferometer. The microfluidic chip platform was developed for this purpose through 3D printing. The Fabry-Perot cavity was incorporated in the microfluidic chip perpendicularly to the sample flow, which was of approximately 3.7 µL/s. The optofluidic fiber sensor platform coupled with a low-cost optical power meter detector was characterized using different concentrations of glucose solutions. In the linear regression analysis, the optical power shift was correlated with the refractive index and a sensitivity of -86.6 dB/RIU (r2 = 0.996) was obtained. Good results were obtained in terms of stability with a maximum standard deviation of 0.03 dB and a sensor resolution of 5.2 × 10-4 RIU. The feasibility of the optofluidic fiber sensor for dynamic analyses of refractive index with low sample usage was confirmed through real-time measurements.

Optical Fiber Sensor for Monitoring the Evaporation of Ethanol-Water Mixtures.

An inline optical fiber sensor is proposed to monitor in real time the evaporation process of ethanol-water binary mixtures. The sensor presents two interferometers, a cladding modal interferometer (CMI) and a Mach-Zehnder interferometer (MZI). The CMI is used to acquire the variations in the external medium refractive index, presenting a maximum sensitivity of 387 nm/RIU, and to attain the variation in the sample concentration profile, while the MZI monitors temperature fluctuations. For comparison purposes, an image analysis is also conducted to obtain the droplet profile. The sensor proposed in this work is a promising alternative in applications where a rigorous measurement of volatile organic compound concentrations is required, and in the study of chemical and physical properties related to the evaporation process.

Is Sotolon Relevant to the Aroma of Madeira Wine Blends?

Madeira wine (MW) oxidative aging results in the formation of several key aromas. Little is still known about their odor relevance to the aroma of the most commercialized MWs. This report presents an in-depth study of the odor impact of sotolon in MW blends. First, its odor perception was estimated in MWs according to ASTM E679, testing different 3-year-old (3-yo) commercial blends. The odor relevance of sotolon in the aroma of 3-, 5-, and 10-yo commercial blends (89 MWs) was then appraised by calculating its Odor Activity Value (OAV), after determining its content by RP-HPLC-MS/MS. The sotolon odor perception in MW was as low as 23 µg/L, although it was found that little differences in the wine matrix influenced its perception. OAVs varied between 0.1 and 22, increasing with the blend age. Considering that 16% of the OAVs are higher than 10 (mostly ≥ 10-yo), sotolon was found to be a key contributor to the overall aroma MW blends.

Rapid Determination of Sotolon in Fortified Wines Using a Miniaturized Liquid-Liquid Extraction Followed by LC-MS/MS Analysis.

Sotolon (4,5-dimethyl-3-hydroxy-2,5-dihydrofuran-2-one) is a powerful odorant usually pointed out as being responsible not only for the characteristic curry notes of the finest fortified wines but also for the off-flavour notes in prematurely oxidized white wines. Most methods reported in literature for quantifying sotolon in wines are quite laborious and use large volumes of organic solvents. Thus, in the present study, the development of a simple, fast, and environment-friendly method for the quantification of sotolon in fortified wine is herein presented. The proposed method uses a single-step liquid-liquid extraction followed by RP-LC-MS/MS and was optimized using a full factorial design. The method showed good linearity (R 2 = 0.9999), intra- and interday precision lower than 10% RSD, recovery of about 95%, and high sensitivity (LOQ of 0.04 µg/L). The method was applied to analyse 44 fortified wines from different styles (from dry to sweet wines) and ages (3-115 years old), and it was found that it covers the concentration range usually found for this compound in this kind of alcoholic beverages, which was found to be within 6.3-810 µg/L. Thus, it can be concluded that this method can be used as an accurate tool for the rapid analysis of sotolon, since the early stages of its formation up to long ageing periods.

Volatile profile of Madeira wines submitted to traditional accelerated ageing.

The evolution of monovarietal fortified Madeira wines forced-aged by traditional thermal processing (estufagem) were studied in terms of volatiles. SPE extracts were analysed by GC-MS before and after heating at 45 °C for 3 months (standard) and at 70 °C for 1 month (overheating). One hundred and ninety volatile compounds were identified, 53 of which were only encountered in baked wines. Most chemical families increased after standard heating, especially furans and esters, up to 61 and 3-fold, respectively. On the contrary, alcohols, acetates and fatty acids decreased after heating. Varietal aromas, such as Malvasia's monoterpenic alcohols were not detected after baking. The accelerated ageing favoured the development of some volatiles previously reported as typical aromas of finest Madeira wines, particularly phenylacetaldeyde, ß-damascenone and 5-ethoxymethylfurfural. Additionally, ethyl butyrate, ethyl 2-methylbutyrate, ethyl caproate, ethyl isovalerate, guaiacol, 5-hydroxymethylfurfural and γ-decalactone were also found as potential contributors to the global aroma of baked wines.

Rapid and sensitive methodology for determination of ethyl carbamate in fortified wines using microextraction by packed sorbent and gas chromatography with mass spectrometric detection.

This work presents a new methodology to quantify ethyl carbamate (EC) in fortified wines. The presented approach combines the microextraction by packed sorbent (MEPS), using a hand-held automated analytical syringe, with one-dimensional gas chromatography coupled with mass spectrometry detection (GC-MS). The performance of different MEPS sorbent materials was tested, namely SIL, C2, C8, C18, and M1. Also, several extraction solvents and the matrix effect were evaluated. Experimental data showed that C8 and dichloromethane were the best sorbent/solvent pair to extract EC. Concerning solvent and sample volumes optimization used in MEPS extraction an experimental design (DoE) was carried out. The best extraction yield was achieved passing 300 µL of sample and 100 µL of dichloromethane. The method validation was performed using a matrix-matched calibration using both sweet and dry fortified wines, to minimize the matrix effect. The proposed methodology presented good linearity (R(2)=0.9999) and high sensitivity, with quite low limits of detection (LOD) and quantification (LOQ), 1.5 µg L(-1) and 4.5 µg L(-1), respectively. The recoveries varied between 97% and 106%, while the method precision (repeatability and reproducibility) was lower than 7%. The applicability of the methodology was confirmed through the analysis of 16 fortified wines, with values ranging between 7.3 and 206 µg L(-1). All chromatograms showed good peak resolution, confirming its selectivity. The developed MEPS/GC-MS methodology arises as an important tool to quantify EC in fortified wines, combining efficiency and effectiveness, with simpler, faster and affordable analytical procedures that provide great sensitivity without using sophisticated and expensive equipment.

Polyphenols, antioxidant potential and color of fortified wines during accelerated ageing: the Madeira Wine case study.

Polyphenols, antioxidant potential and color of three types of fortified Madeira wines were evaluated during the accelerated ageing, named as estufagem. The traditional estufagem process was set to 45 °C for 3 months. Overheating conditions, 1 month at 70 °C, were also examined. Total polyphenols (TP), total monomeric anthocyanins (TMA) and total flavonoids (TF) were assessed by spectrophotometric methods, while individual polyphenols and furans were simultaneously determined by HPLC-DAD. Antioxidant potential (AP) was estimated by ABTS, DPPH and FRAP assays, while color was evaluated by Glories and CIELab. Traditional estufagem decreased the TP and AP up to 20% and 26%, respectively, with final values similar to other wines. TMA of the Madeira wines from red grapes decreased during estufagem. Six hydroxybenzoic acids, three hydroxycinnamic acids, one stilbene, three flavonols and three flavan-3-ols were found in these wines. The prominent phenolics were hydroxycinnamates and hydroxybenzoates, even after estufagem. Most polyphenols decreased, with the exception of caffeic, ferulic, p-coumaric, gallic and syringic acids. Finally, both chromatic systems revealed that all wines tended to similar chromatic characteristics after estufagem. The study suggests that estufagem can be applied without high impact on polyphenols and antioxidant potential of these fortified wines.

Determination of toxic elements in coal by ICP-MS after digestion using microwave-induced combustion.

A microwave-induced combustion (MIC) procedure was applied for coal digestion for subsequent determination of As, Cd and Pb by inductively coupled plasma mass spectrometry (ICP-MS) and Hg using cold vapor (CV) generation coupled to ICP-MS. Pellets of coal (500 mg) were combusted using 20 bar of oxygen and ammonium nitrate as aid for ignition. The use of nitric acid as absorbing solution (1.7, 3.5, 5.0, 7.0 and 14 mol L(-1)) was evaluated. For coal samples with higher ash content, better results were found using 7.0 mol L(-1) HNO(3) and an additional reflux step of 5 min after combustion step. For coal samples with ash content lower than 8%, 5.0 mol L(-1) nitric acid was suitable to the absorption of all analytes. Accuracy was evaluated using certified reference material (CRM) of coal and spikes. Agreement with certified values and recoveries was better than 95 and 97%, respectively, for all the analytes. For comparison of results, a procedure recommended by the American Society of Testing and Materials (ASTM) was used. Additionally, a conventional microwave-assisted digestion (MAD) in pressurized vessels was also performed. Using ASTM procedure, analyte losses were observed and a relatively long time was necessary for digestion (>6h). By comparison with MAD procedure, higher sample mass can be digested using MIC allowing better limits of detection. Additionally, the use of concentrated acids was not necessary that is an important aspect in order to obtain low blank levels and lower limits of detection, respectively. The residual carbon content in digests obtained by MAD and MIC was about 15% and <1%, respectively, showing the better digestion efficiency of MIC procedure. Using MIC it was possible to digest completely and simultaneously up to eight samples in only 25 min with relatively lower generation of laboratory effluents.

HPLC-DAD methodology for the quantification of organic acids, furans and polyphenols by direct injection of wine samples.

This article proposes a simple and sensitive HPLC method with photo-diode array detection for the analysis of organic acids, monomeric polyphenols and furanic compounds in wine samples by direct injection. The chromatographic separation of 8 organic acids, 2 furans and 22 phenolic compounds was carried out with a buffered solution (pH 2.70) and acetonitrile as mobile phases and a difunctionally bonded C18 stationary phase, Atlantis dC18 (250x4.6 mm, 5 mum) column. The elution was performed in 12 min for the organic acids and in 60 min for the phenolic compounds, including phenolic acids, stilbenes and flavonoids. Target compounds were detected at 210 nm (organic acids, flavan-3-ols and benzoic acids), 254 nm (ellagic acid), 280 nm (furans and cinnamic acid), 315 nm (hydroxycinnamic acids and trans-resveratrol) and 360 nm (flavonoids). The RSD for the repeatability test (n=5) of peak area and retention times were below 3.1 and 0.3%, respectively, for phenolics and below 1.0 and 0.2% for organic acids. The RSDs expressing the reproducibility of the method were higher than for the repeatability results but all below 9.0%. Method accuracy was evaluated by the recovery results, with averaged values between 80 and 104% for polyphenols and 97-105% for organic acids. The calibration curves, obtained by triplicate injection of standard solutions, showed good linearity with regression coefficients higher than 0.9982 for polyphenols and 0.9997 for organic acids. The LOD was in the range of 0.07-0.49 mg/L for polyphenols (cinnamic and gallic acids, respectively) and 0.001-0.046 g/L for organic acids (oxalic and lactic acids, respectively). The method was successfully used to measure and assess the polyphenolic fingerprint and organic acids profile of red, white, rosé and fortified wines.

Quantification of polyphenols with potential antioxidant properties in wines using reverse phase HPLC.

A RP-HPLC method with photodiode array detection (DAD) was developed to separate, identify and quantify simultaneously the most representative phenolic compounds present in Madeira and Canary Islands wines. The optimized chromatographic method was carefully validated in terms of linearity, precision, accuracy and sensitivity. A high repeatability and a good stability of phenolics retention times (< 3%) were obtained, as well as relative peak area. Also high recoveries were achieved, over 80.3%. Polyphenols calibration curves showed a good linearity (r(2) >0.994) within test ranges. Detection limits ranged between 0.03 and 11.5 microg/mL for the different polyphenols. A good repeatability was obtained, with intra-day variations less than 7.9%. The described method was successfully applied to quantify several polyphenols in 26 samples of different kinds of wine (red, rosé and white wines) from Madeira and Canary Islands. Gallic acid was by far the most predominant acid. It represents more than 65% of all phenolics, followed by p-coumaric and caffeic acids. The major flavonoid found in Madeira wines was trans-resveratrol. In some wines, (-)-epicatechin was also found in highest amount. Canary wines were shown to be rich in gallic, caffeic and p-coumaric acids and quercetin.

Psicanálise e psiquiatria: diálogo possível?

A parir de referências literárias (Kafka, Dante) e científicas, a autora faz algumas reflexões, procurando delimitar um campo Ético no qual a Psicanálise e a Psiquiatria poderiam estabelecer um dialogo passível

Interpretação: entre uma perda e um ganho?

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Psicanálise/Fenômeno Psicossomático/Idoso

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