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.

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.

Optimal design of experiments applied to headspace solid phase microextraction for the quantification of vicinal diketones in beer through gas chromatography-mass spectrometric detection.

Vicinal diketones, namely diacetyl (DC) and pentanedione (PN), are compounds naturally found in beer that play a key role in the definition of its aroma. In lager beer, they are responsible for off-flavors (buttery flavor) and therefore their presence and quantification is of paramount importance to beer producers. Aiming at developing an accurate quantitative monitoring scheme to follow these off-flavor compounds during beer production and in the final product, the head space solid-phase microextraction (HS-SPME) analytical procedure was tuned through experiments planned in an optimal way and the final settings were fully validated. Optimal design of experiments (O-DOE) is a computational, statistically-oriented approach for designing experiences that are most informative according to a well-defined criterion. This methodology was applied for HS-SPME optimization, leading to the following optimal extraction conditions for the quantification of VDK: use a CAR/PDMS fiber, 5 ml of samples in 20 ml vial, 5 min of pre-incubation time followed by 25 min of extraction at 30 °C, with agitation. The validation of the final analytical methodology was performed using a matrix-matched calibration, in order to minimize matrix effects. The following key features were obtained: linearity (R(2) > 0.999, both for diacetyl and 2,3-pentanedione), high sensitivity (LOD of 0.92 µg L(-1) and 2.80 µg L(-1), and LOQ of 3.30 µg L(-1) and 10.01 µg L(-1), for diacetyl and 2,3-pentanedione, respectively), recoveries of approximately 100% and suitable precision (repeatability and reproducibility lower than 3% and 7.5%, respectively). The applicability of the methodology was fully confirmed through an independent analysis of several beer samples, with analyte concentrations ranging from 4 to 200 g L(-1).

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.