Browsing by Author "Rodrigues, Freddy"
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- DLLμE/GC-MS as a Powerful Analytical Approach to Establish the Volatilomic Composition of Different WhiskeysPublication . Perestrelo, Rosa; Caldeira, Michael; Rodrigues, Freddy; Pereira, Jorge A. M.; Câmara, José S.The volatilomic fingerprint of nine different whiskeys was established using a rapid and sensitive analytical approach based on dispersive liquid–liquid microextraction (DLLµE) followed by gas chromatography mass spectrometry detection (GC-MS) and gas chromatography with flame ionization detection (GC-FID). The influence of the extractor solvent on the extraction efficiency of volatile compounds (VOCs) was evaluated by DLLµE/GC-MS. The highest amounts of VOCs were obtained using 5 mL of sample, dichloromethane as the extractor solvent, and acetone as the disperser solvent. The proposed method showed no matrix effect, good linearity (R2 ≥ 0.993) in the assessed concentration range, recovery (ranging from 70 to 99%, precision (RSD ≤ 15%) and sensitivity (low limits of detection and quantification). A total of 37 VOCs belonging to different biosynthetic pathways including alcohols, esters, acids, carbonyl compounds, furanic compounds and volatile phenols were identified and quantified using DLLµE/GC-MS and DLLµE/GC-FID, respectively. Alcohols (3-methylbutan-1-ol, propan-1-ol), esters (ethyl decanoate, ethyl octanoate, ethyl hexanoate), and acids (decanoic acid, octanoic acid, hexanoic acid) were the most abundant chemical families. The multivariate statistical analysis allowed for the discrimination of whiskeys based on their volatilomic fingerprint, namely octanoic acid, 2-furfural, ethyl octanoate, ethyl hexanoate, acetic acid, ethyl dodecanoate, butan-1-ol, and ethyl decanoate.
- New uses for old drugs: pharmacophore‐based screening for the discovery of P‐glycoprotein inhibitorsPublication . Palmeira, Andreia; Rodrigues, Freddy; Sousa, Emília; Pinto, Madalena; Vasconcelos, M. Helena; Fernandes, Miguel X.P-glycoprotein (P-gp) is one of the best character ized transporters responsible for the multidrug resistance phenotype exhibited by cancer cells. Therefore, there is widespread interest in eluci dating whether existing drugs are candidate P-gp substrates or inhibitors. With this aim, a pharma cophore model was created based on known P-gp inhibitors and it was used to screen a database of existing drugs. The P-gp modulatory activity of the best hits was evaluated by several methods such as the rhodamine-123 accumulation assay using K562Dox cell line, and a P-gp ATPase activ ity assay. The ability of these compounds to enhance the cytotoxicity of doxorubicin was assessed with the sulphorhodamine-B assay. Of the 21 hit compounds selected in silico, 12 were found to significantly increase the intracellular accumulation of Rhodamine-123, a P-gp substrate. In addition, amoxapine and loxapine, two tetracy clic antidepressant drugs, were discovered to be potent non-competitive inhibitors of P-gp, causing a 3.5-fold decrease in the doxorubicin GI50 in K562Dox cell line. The overall results provide important clues for the non-label use of known drugs as inhibitors of P-gp. Potent inhibitors with a dibenzoxazepine scaffold emerged from this study and they will be further investigated in order to develop new P-gp inhibitors.
- Volatile flavour constituent patterns of terras madeirenses red wines extracted by dynamic headspace solid‐phase microextractionPublication . Perestrelo, Rosa Maria de Sá; Caldeira, Michael Manuel Lima; Rodrigues, FreddyA suitable analytical procedure based on static headspace solid-phase microextraction (SPME) followed by thermal desorption gas chromatography–ion trap mass spectrometry detection (GC–ITDMS), was developed and applied for the qualitative and semi-quantitative analysis of volatile components of Portuguese Terras Madeirenses red wines. The headspace SPME method was optimised in terms of fibre coating, extraction time, and extraction temperature. The performance of three commercially available SPME fibres, viz. 100 lm polydimethylsiloxane; 85 lm polyacrylate, PA; and 50/30 lm divinylbenzene/carboxen on polydimethylsiloxane, was evaluated and compared. The highest amounts extracted, in terms of the maximum signal recorded for the total volatile composition, were obtained with a PA coating fibre at 308C during an extraction time of 60 min with a constant stirring at 750 rpm, after saturation of the sample with NaCl (30%, w/v). More than sixty volatile compounds, belonging to different biosynthetic pathways, have been identified, including fatty acid ethyl esters, higher alcohols, fatty acids, higher alcohol acetates, isoamyl esters, carbonyl compounds, and monoterpenols/C13-norisoprenoids.