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Prof. José Sousa Câmara
University of Madeira

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0 Metabolomics
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Original article
Published: 13 August 2021 in Metabolomics
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Globally, breast cancer (BC) is leading at the top of women's diseases and, as a multifactorial disease, there is the need for the development of new approaches to aid clinicians on monitoring BC treatments. In this sense, metabolomic studies have become an essential tool allowing the establishment of interdependency among metabolites in biological samples. The combination of nuclear magnetic resonance (NMR) and gas chromatography–quadrupole mass spectrometry (GC–qMS) based metabolomic analyses of urine and breast tissue samples from BC patients and cancer-free individuals was used. Multivariate statistical tools were used in order to obtain a panel of metabolites that could discriminate malignant from healthy status assisting in the diagnostic field. Urine samples (n = 30), cancer tissues (n = 30) were collected from BC patients, cancer-free tissues were resected outside the tumor margin from the same donors (n = 30) while cancer-free urine samples (n = 40) where obtained from healthy subjects and analysed by NMR and GC–qMS methodologies. The orthogonal partial least square discriminant analysis model showed a clear separation between BC patients and cancer-free subjects for both classes of samples. Specifically, for urine samples, the goodness of fit (R2Y) and predictive ability (Q2) was 0.946 and 0.910, respectively, whereas for tissue was 0.888 and 0.813, revealing a good predictable accuracy. The discrimination efficiency and accuracy of tissue and urine metabolites was ascertained by receiver operating characteristic curve analysis that allowed the identification of metabolites with high sensitivity and specificity. The metabolomic pathway analysis identified several dysregulated pathways in BC, including those related with lactate, valine, aspartate and glutamine metabolism. Additionally, correlations between urine and tissue metabolites were investigated and five metabolites (e.g. acetone, 3-hexanone, 4-heptanone, 2-methyl-5-(methylthio)-furan and acetate) were found to be significant using a dual platform approach. Overall, this study suggests that an improved metabolic profile combining NMR and GC–qMS may be useful to achieve more insights regarding the mechanisms underlying cancer.

ACS Style

Catarina Luís Silva; Rosa Perestrelo; Filipa Capelinha; Helena Tomás; José S. Câmara. An integrative approach based on GC–qMS and NMR metabolomics data as a comprehensive strategy to search potential breast cancer biomarkers. Metabolomics 2021, 17, 1 -11.

AMA Style

Catarina Luís Silva, Rosa Perestrelo, Filipa Capelinha, Helena Tomás, José S. Câmara. An integrative approach based on GC–qMS and NMR metabolomics data as a comprehensive strategy to search potential breast cancer biomarkers. Metabolomics. 2021; 17 (8):1-11.

Chicago/Turabian Style

Catarina Luís Silva; Rosa Perestrelo; Filipa Capelinha; Helena Tomás; José S. Câmara. 2021. "An integrative approach based on GC–qMS and NMR metabolomics data as a comprehensive strategy to search potential breast cancer biomarkers." Metabolomics 17, no. 8: 1-11.

Journal article
Published: 10 July 2021 in Molecules
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In this study, the health-promoting benefits of different fruits grown in Madeira Island, namely lemon (Citrus limon var. eureka), tangerine (Citrus reticulata var. setubalense), pitanga (Eugenia uniflora var. red), tomato (Solanum lycopersicum var. gordal) and uva-da-serra, an endemic blueberry (Vaccinium padifolium Sm.), were investigated. The phenolic composition (total phenolics and total flavonoids content) and antioxidant capacity (assessed through ABTS and DPPH assays) were measured revealing a high phenolic potential for all fruits, except tomato, while uva-da-serra is particularly rich in flavonoids. In relation to the antioxidant capacity, the highest values were obtained for pitanga and uva-da-serra extracts. The bioactive potential was also assessed through the ability of the extracts to inhibit digestive enzymes linked to diabetes (α-amylase, α- and β-glucosidases) and hypertension (angiotensin-converting enzyme, ACE). The results obtained point to a very high bioactive potential with the selected samples exhibiting very important ACE anti-enzymatic capacities. A statistical analysis of the obtained data reveals a very strong correlation between ABTS and TPC, and a strong contribution of the fruit polyphenols for enzyme inhibition, and thus, presenting high antihypertensive and antidiabetic capacities. Overall, the results obtained clearly show a high bioactive potential of the selected fruits that should be further studied, in terms of specific phenolic composition. Moreover, these results strongly support the valorisation of pitanga seeds usually discarded as a waste, and uva-da-serra, an endemic and wild bush, as potential bioresources of bioactive compounds with impact in human diet.

ACS Style

José Figueira; Priscilla Porto-Figueira; Cristina Berenguer; Jorge Pereira; José Câmara. Evaluation of the Health-Promoting Properties of Selected Fruits. Molecules 2021, 26, 4202 .

AMA Style

José Figueira, Priscilla Porto-Figueira, Cristina Berenguer, Jorge Pereira, José Câmara. Evaluation of the Health-Promoting Properties of Selected Fruits. Molecules. 2021; 26 (14):4202.

Chicago/Turabian Style

José Figueira; Priscilla Porto-Figueira; Cristina Berenguer; Jorge Pereira; José Câmara. 2021. "Evaluation of the Health-Promoting Properties of Selected Fruits." Molecules 26, no. 14: 4202.

Journal article
Published: 05 July 2021 in Foods
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Sugarcane honey (SCH) is a syrup produced on Madeira Island and recognized by its unique aroma, a complex attribute of quality with an important influence on the final consumer’s acceptance of the product, and determined by a complex mixture of a large number of volatile organic compounds (VOCs) generated during its traditional making process and storage. Therefore, the purpose of this study was to establish the volatile profile of genuine SCH produced by a regional certified producer for seven years and compare it with syrups from non-certified regional producers and with producers from different geographical regions (Spain, Egypt, Brazil and Australia), as a powerful strategy to define the volatomic fingerprint of SCH. Different volatile profiles were recognized for all samples, with 166 VOCs being identified belonging to different chemical classes, including furans, ketones, carboxylic acids, aldehydes and alcohols. Chemometric analysis allowed (i) the differentiation between all syrups, being more pronounced between SCH and other syrups; and (ii) the identification of 32 VOCs as potential markers for the traceability and authenticity of SCH on the global market.

ACS Style

Pedro Silva; Jorge Freitas; Fernando Nunes; José Câmara. A Predictive Strategy Based on Volatile Profile and Chemometric Analysis for Traceability and Authenticity of Sugarcane Honey on the Global Market. Foods 2021, 10, 1559 .

AMA Style

Pedro Silva, Jorge Freitas, Fernando Nunes, José Câmara. A Predictive Strategy Based on Volatile Profile and Chemometric Analysis for Traceability and Authenticity of Sugarcane Honey on the Global Market. Foods. 2021; 10 (7):1559.

Chicago/Turabian Style

Pedro Silva; Jorge Freitas; Fernando Nunes; José Câmara. 2021. "A Predictive Strategy Based on Volatile Profile and Chemometric Analysis for Traceability and Authenticity of Sugarcane Honey on the Global Market." Foods 10, no. 7: 1559.

Journal article
Published: 02 July 2021 in Food Research International
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Uveira-da-serra (Vaccinium padifolium Sm) is a native blueberry from Madeira Island (Portugal). In this study, the free low-molecular weight phenolic composition of Vaccinium padifolium berries (uva-da-serra - UdS), was established using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) strategy combined with liquid chromatography electrospray ionization tandem mass spectroscopy (LC-ESI-MSMS). Total phenolic content (TPC), total flavonoid content (TFC), 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid (ABTS) radical-scavenging activities and oxygen radical absorbance capacity (ORAC) were also evaluated. Twenty-six phenolic compounds were identified in the UdS, being chlorogenic acid (17.4 mg/g DW), epigallocatechin (2.33 mg/g DW), caffeic acid (0.66 mg/g DW), quercetin-3-glucoside (0.38 mg/g DW) and myricetin (0.33 mg/g DW) the predominant compounds. As far we are aware, this is the first time that the free low molecular weight phenolic composition of Vaccinium padifolium Sm is characterized, also unveiling (-)epigallocatechin gallate, o-coumaric acid and m-coumaric acids presence in a Vaccinium specie. TPC (3021.8 mg GAE/100g DW), TFC (2645.2 mg QE/100g DW), DPPH (20509.0 µmol TE/g DW), ORAC (18510.0 µmol TE/g DW) and ABTS (19338.0 µmol TE/g DW) suggest a high antioxidant potential which is to health benefits including on cardiovascular and neurodegenerative disease prevention, , making UdS a useful biosource with potential applications in food, pharmaceutical and cosmetic industries.

ACS Style

José A. Figueira; Priscilla Porto-Figueira; Jorge A. M. Pereira; José S. Câmara. Free low-molecular weight phenolics composition and bioactivity of Vaccinium padifolium Sm fruits. Food Research International 2021, 148, 110580 .

AMA Style

José A. Figueira, Priscilla Porto-Figueira, Jorge A. M. Pereira, José S. Câmara. Free low-molecular weight phenolics composition and bioactivity of Vaccinium padifolium Sm fruits. Food Research International. 2021; 148 ():110580.

Chicago/Turabian Style

José A. Figueira; Priscilla Porto-Figueira; Jorge A. M. Pereira; José S. Câmara. 2021. "Free low-molecular weight phenolics composition and bioactivity of Vaccinium padifolium Sm fruits." Food Research International 148, no. : 110580.

Review
Published: 01 July 2021 in Toxics
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Phthalates are a group of chemicals used in a multitude of important industrial products (e.g., medical devices, children’s toys, and food packages), mainly as plasticizers to improve mechanical properties such as flexibility, transparency, durability, and longevity of polyvinyl chloride (PVC). The wide occurrence of phthalates in many consumer products, including foods (e.g., bottled water, soft drinks, wine, milk, and meat) brings that most people are exposed to phthalates every day, which raises some concerns. Adverse health outcomes from phthalates exposure have been associated with endocrine disruption, deformities in the human reproductive system, increased risk of preterm birth, carcinogen exposure, among others. Apprehension related to the health risks and ubiquitous incidence of phthalates in foods inspires the development of reliable analytical approaches that allow their detection and quantification at trace levels. The purpose of the current review is to provide information related to the presence of phthalates in the food chain, highlighting the health risks associated with their exposure. Moreover, an overview of emerging extraction procedures and high-resolution analytical approaches for a comprehensive quantification of phthalates is presented.

ACS Style

Catarina Luís; Manuel Algarra; José Câmara; Rosa Perestrelo. Comprehensive Insight from Phthalates Occurrence: From Health Outcomes to Emerging Analytical Approaches. Toxics 2021, 9, 157 .

AMA Style

Catarina Luís, Manuel Algarra, José Câmara, Rosa Perestrelo. Comprehensive Insight from Phthalates Occurrence: From Health Outcomes to Emerging Analytical Approaches. Toxics. 2021; 9 (7):157.

Chicago/Turabian Style

Catarina Luís; Manuel Algarra; José Câmara; Rosa Perestrelo. 2021. "Comprehensive Insight from Phthalates Occurrence: From Health Outcomes to Emerging Analytical Approaches." Toxics 9, no. 7: 157.

Journal article
Published: 01 July 2021 in Food Chemistry
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Sugarcane honey (SCH) is a syrup from Madeira Island recognized by its unique and excellent aroma, associated to volatile organic compounds (VOCs) generated during the well-defined five stages of its traditional making process. The establishment of volatile profile throughout all SCH-making stages during four years, allowed the evaluation of the influence of each stage in the typical characterisitcs of SCH. One hundred eighthy seven VOCs were identified, being associated to several origins and formation pathways. VOCs formed during stage 1 and 2 were originate from raw material, and its oxidation (i.e. enzymatic browning) and thermal degradation (i.e. lipid oxidation, Maillard reactions, Strecker degradation). In stage 3 and 4, the caramelization and melanoidin degradation also occurred, while in stage 5, the thermal degradation continues, followed by microbial activity. Chemometric analysis allowed to identify 35 VOCs as potential markers for processing control by the producers and as guarantee of the typicality and authenticity of SCH. Based on the obtained results, we propose for the first time an innovative schematic diagram explaining the potential reactions and pathways for VOCs formation during the different steps of the SCH production.

ACS Style

Pedro Silva; Jorge Freitas; Fernando M. Nunes; José S. Câmara. Effect of processing and storage on the volatile profile of sugarcane honey: A four-year study. Food Chemistry 2021, 365, 130457 .

AMA Style

Pedro Silva, Jorge Freitas, Fernando M. Nunes, José S. Câmara. Effect of processing and storage on the volatile profile of sugarcane honey: A four-year study. Food Chemistry. 2021; 365 ():130457.

Chicago/Turabian Style

Pedro Silva; Jorge Freitas; Fernando M. Nunes; José S. Câmara. 2021. "Effect of processing and storage on the volatile profile of sugarcane honey: A four-year study." Food Chemistry 365, no. : 130457.

Review
Published: 01 July 2021 in Separations
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Some chemical substances have the potential to enter the coastal and marine environment and cause adverse effects on ecosystems, biodiversity and human health. For a large majority of them, their fate and effects are poorly understood as well as their use still unregulated. Finding effective and sustainable strategies for the identification of these emerging and/or anthropogenic contaminants that might cause polluting effects in marine environments to mitigate their adverse effects, is of utmost importance and a great challenge for managers, regulators and researchers. In this review we will evaluate the impact of emerging contaminants (ECs) on marine coastal zones namely in their ecosystems and biodiversity, highlighting the potential risks of organic pollutants, pharmaceuticals and personal care products. Emerging microextraction techniques and high-resolution analytical platforms used in isolation, identification and quantification of ECs will be also reviewed.

ACS Style

José Câmara; Sarah Montesdeoca-Esponda; Jorge Freitas; Rayco Guedes-Alonso; Zoraida Sosa-Ferrera; Rosa Perestrelo. Emerging Contaminants in Seafront Zones. Environmental Impact and Analytical Approaches. Separations 2021, 8, 95 .

AMA Style

José Câmara, Sarah Montesdeoca-Esponda, Jorge Freitas, Rayco Guedes-Alonso, Zoraida Sosa-Ferrera, Rosa Perestrelo. Emerging Contaminants in Seafront Zones. Environmental Impact and Analytical Approaches. Separations. 2021; 8 (7):95.

Chicago/Turabian Style

José Câmara; Sarah Montesdeoca-Esponda; Jorge Freitas; Rayco Guedes-Alonso; Zoraida Sosa-Ferrera; Rosa Perestrelo. 2021. "Emerging Contaminants in Seafront Zones. Environmental Impact and Analytical Approaches." Separations 8, no. 7: 95.

Journal article
Published: 15 June 2021 in Molecules
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In recent years, there has been a growing interest in studying and exploring the potential health benefits of foods, mainly from vegetables and fruits from regular intake. The presence of secondary metabolites, namely polyphenols, carotenoids and terpenes, in certain food matrices seems to contribute to their functional properties, expressed through an increased prevention in the development of certain chronic diseases, namely coronary heart diseases, neurodegenerative diseases, cancer and diabetes. However, some foods’ volatile secondary metabolites also present important bioactive properties, although this is a poorly scientifically explored field. In this context, and in order to explore the potential bioactivity of volatile metabolites in different vegetables and fruits from regular consumption, the volatile composition was established using a green extraction technique, solid phase microextraction in headspace mode (HS-SPME), combined with gas chromatography tandem mass spectrometry (GC-MS). A total of 320 volatile metabolites, comprising 51 terpenic compounds, 45 organosulfur compounds, 31 aldehydes, 37 esters, 29 ketones, 28 alcohols, 23 furanic compounds, 22 hydrocarbons, 19 benzene compounds, 13 nitrogenous compounds, 9 carboxylic acids, 7 ethers, 4 halogenated compounds and 3 naphthalene derivatives, were positively identified. Each investigated fruit and vegetable showed a specific volatile metabolomic profile. The obtained results revealed that terpenic compounds, to which are associated antimicrobial, antioxidant, and anticancer activities, are the most predominant chemical family in beetroot (61%), orange carrot (58%) and white carrot (61%), while organosulfur compounds (antiviral activity) are dominant in onion, garlic and watercress. Broccoli and spinach are essentially constituted by alcohols and aldehydes (enzyme-inhibition and antimicrobial properties), while fruits from the Solanaceae family are characterized by esters in tamarillo and aldehydes in tomato.

ACS Style

Joselin Aguiar; João Gonçalves; Vera Alves; José Câmara. Relationship between Volatile Composition and Bioactive Potential of Vegetables and Fruits of Regular Consumption—An Integrative Approach. Molecules 2021, 26, 3653 .

AMA Style

Joselin Aguiar, João Gonçalves, Vera Alves, José Câmara. Relationship between Volatile Composition and Bioactive Potential of Vegetables and Fruits of Regular Consumption—An Integrative Approach. Molecules. 2021; 26 (12):3653.

Chicago/Turabian Style

Joselin Aguiar; João Gonçalves; Vera Alves; José Câmara. 2021. "Relationship between Volatile Composition and Bioactive Potential of Vegetables and Fruits of Regular Consumption—An Integrative Approach." Molecules 26, no. 12: 3653.

Review
Published: 29 May 2021 in Foods
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For centuries, wine has had a fundamental role in the culture and habits of different civilizations. Amongst numerous wine types that involve specific winemaking processes, fortified wines possess an added value and are greatly honored worldwide. This review comprises the description of the most important characteristics of the main worldwide fortified wines—Madeira, Port, Sherry, Muscat, and Vermouth—structured in three parts. The first part briefly describes the chemistry of wine flavor, the origin of typical aroma (primary, secondary and tertiary), and the influencing parameters during the winemaking process. The second part describes some specificities of worldwide fortified wine, highlighting the volatile composition with particular emphasis on aroma compounds. The third part reports the volatile composition of the most important fortified wines, including the principal characteristics, vinification process, the evolution of volatile organic compounds (VOCs) during the aging processes, and the most important odor descriptors. Given the worldwide popularity and the economic relevance of fortified wines, much research should be done to better understand accurately the reactions and mechanisms that occur in different stages of winemaking, mainly during the oxidative and thermal aging.

ACS Style

Teresa Abreu; Rosa Perestrelo; Matteo Bordiga; Monica Locatelli; Jean Daniel Coïsson; José Câmara. The Flavor Chemistry of Fortified Wines—A Comprehensive Approach. Foods 2021, 10, 1239 .

AMA Style

Teresa Abreu, Rosa Perestrelo, Matteo Bordiga, Monica Locatelli, Jean Daniel Coïsson, José Câmara. The Flavor Chemistry of Fortified Wines—A Comprehensive Approach. Foods. 2021; 10 (6):1239.

Chicago/Turabian Style

Teresa Abreu; Rosa Perestrelo; Matteo Bordiga; Monica Locatelli; Jean Daniel Coïsson; José Câmara. 2021. "The Flavor Chemistry of Fortified Wines—A Comprehensive Approach." Foods 10, no. 6: 1239.

Journal article
Published: 23 March 2021 in Microchemical Journal
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Electronic cigarettes (e-cigarettes) have become popular alternatives to traditional tobacco. Despite this, a comprehensive evaluation of their long-term effects and safety for the consumers and the environment is missing. To contribute to filling this gap, headspace solid-phase microextraction combined with gas chromatography-mass spectrometry (HS-SPME/GC–MS) was employed to establish and compare the volatile fingerprints of traditional tobacco and e-cigarettes. The analysis of traditional tobacco included two popular brands and different parts of the cigarette (solid tobacco, cigarette smoke, cigarette paper and filter). Regarding the e-cigarettes, two e-liquids, with and without nicotine, their main constituents (e-bases) and corresponding vapours, obtained under default vaping (power) conditions, were analysed. A total of 80 volatile organic compounds (VOCs) were identified in traditional tobacco, of which 14 carbonyl compounds, 9 benzene derivatives, 9 ethyl esters and 9 hydrocarbons. Slight differences in the volatile profile of cigarette paper and filter between the two brands were also detected, showing that exogenous components of tobacco influence the flavour and harmfulness perceived by the smokers. In turn, 92 VOCs were identified in e-cigarettes, including 31 ethyl esters, 18 alcohols and 10 hydrocarbons. No VOCs with potentially toxic or harmful effects were identified in the vapour of Do It Yourself (DIY) liquids and Premium samples. Therefore, taking into consideration the volatile compositions obtained for smoking and vaping procedures under normal conditions of operation and using certified e-liquid mixtures, the e-cigarettes analysed seemed to constitute a valid and less harmful alternative to traditional tobacco for smokers, second-hand smokers and the environment.

ACS Style

Cristina Berenguer; Jorge A.M. Pereira; José S. Câmara. Fingerprinting the volatile profile of traditional tobacco and e-cigarettes: A comparative study. Microchemical Journal 2021, 166, 106196 .

AMA Style

Cristina Berenguer, Jorge A.M. Pereira, José S. Câmara. Fingerprinting the volatile profile of traditional tobacco and e-cigarettes: A comparative study. Microchemical Journal. 2021; 166 ():106196.

Chicago/Turabian Style

Cristina Berenguer; Jorge A.M. Pereira; José S. Câmara. 2021. "Fingerprinting the volatile profile of traditional tobacco and e-cigarettes: A comparative study." Microchemical Journal 166, no. : 106196.

Research article
Published: 15 March 2021 in Journal of Agricultural and Food Chemistry
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Sugarcane (SC) is a perennial grass widely cultivated in tropical and subtropical regions. However, its cultivation in Europe is residual, where Madeira Island, Portugal, is the only region where SC continues to be extensively cultivated. For the first time, the volatile profiles of regional cultivars were established by solid-phase microextraction combined with gas chromatography–mass spectrometry. Different volatile profiles for each cultivar were recognized, identifying 260 volatile organic compounds belonging to 15 chemical classes, such as aldehydes, alcohols, ketones, hydrocarbons, esters, and terpenes. Chemometric analysis procedure, namely, one-way ANOVA with Tukey’s test, principal component analysis, partial least-square analysis, linear discriminant analysis, and hierarchical clustering analysis, allowed the differentiation between all regional cultivars. This study represents an important contribution for the maintenance of biodiversity and subsistence of the SC industry in Europe. Furthermore, it is also a valuable contribution to establish the typicality of traditional SC-based products, such as SC honey.

ACS Style

Pedro Silva; Jorge Freitas; Fernando M. Nunes; José S. Câmara. Chemical Differentiation of Sugarcane Cultivars Based on Volatile Profile and Chemometric Analysis. Journal of Agricultural and Food Chemistry 2021, 69, 3548 -3558.

AMA Style

Pedro Silva, Jorge Freitas, Fernando M. Nunes, José S. Câmara. Chemical Differentiation of Sugarcane Cultivars Based on Volatile Profile and Chemometric Analysis. Journal of Agricultural and Food Chemistry. 2021; 69 (11):3548-3558.

Chicago/Turabian Style

Pedro Silva; Jorge Freitas; Fernando M. Nunes; José S. Câmara. 2021. "Chemical Differentiation of Sugarcane Cultivars Based on Volatile Profile and Chemometric Analysis." Journal of Agricultural and Food Chemistry 69, no. 11: 3548-3558.

Review article
Published: 11 March 2021 in Trends in Food Science & Technology
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The Quality Index Method (QIM) is a widely used approach for fish sensory grading, based on a structured scaling for freshness measurements, providing information concerning the fish freshness status, as a prediction of the remaining shelf-life for specific species or products. However, its tendency to be used in an oversimplified way and other common misapplications could lead to discredit of a methodology with great potential. Review the principles of QIM methodology, discussing its concept, applications, and understand their limits, as a useful strategy to propose improvements, reinforce its predictive power and consequent acceptability. Key findings and conclusions: QIM methodology is based on a compromise between the number of fish samples necessary and the number of attributes, with sensory relevance in fish spoilage, that allows verifying if quality requirements are fulfilled. However, the assumptions inherent to the method, undermine the reliability of the shelf-life predictions. Determination of the variability associated with assessors, product, and correct structure of datasets for statistical analysis, will improve the predictive power of the method. However, it could lead to an increase in the method complexity that would drive it away from the industry's needs for fast and easily implemented methods.

ACS Style

Jorge Freitas; Paulo Vaz-Pires; José S. Câmara. Quality Index Method for fish quality control: Understanding the applications, the appointed limits and the upcoming trends. Trends in Food Science & Technology 2021, 111, 333 -345.

AMA Style

Jorge Freitas, Paulo Vaz-Pires, José S. Câmara. Quality Index Method for fish quality control: Understanding the applications, the appointed limits and the upcoming trends. Trends in Food Science & Technology. 2021; 111 ():333-345.

Chicago/Turabian Style

Jorge Freitas; Paulo Vaz-Pires; José S. Câmara. 2021. "Quality Index Method for fish quality control: Understanding the applications, the appointed limits and the upcoming trends." Trends in Food Science & Technology 111, no. : 333-345.

Journal article
Published: 02 March 2021 in LWT
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The presence of pesticide residues in animal tissues is a source of public awareness and health concerns. Therefore, to guarantee appropriate food safety and to enforce regulations, efficient, cost-effective and sensitive analytical methods are needed. This study set out to develop and validate a reliable and high-throughput analytical approach for the simultaneous determination of N-methyl carbamates (NMCs) in different parts of pork tissues (kidney, liver and muscle). An innovative sample preparation strategy based on ultrasound assisted QuEChERS extraction (UAE-QuEChERS), instead of manual agitation as original QuEChERS, was evaluated. The NMC insecticides were extracted with acidified (1% acetic acid, v/v) acetonitrile (ACN) and determined by reversed-phase high performance liquid chromatography with fluorescence detection (LC-FLD) after automatic post column derivatization and impurities removal through dispersive solid phase extraction (d-SPE). The separation of NMCs was carried out in a C8 column using H2O:ACN (90:10, v/v) and H2O:ACN (20:80, v/v) as mobile phases. The method showed a good linearity (r2 ≥ 0.991), with recoveries generally between 68.6 and 119%. Method limits of detection (LOD) ranging from 0.1 to 2 μg/kg, and method limits of quantification (LOQ) from 0.4 to 6 μg/kg, are satisfactory in terms of the maximum residue limits (MRLs) for NMCs. Suitable intra- and inter-day variations (RSD <12%) and low matrix effects were observed with sample-to-sample variation, for all assayed pork tissues. The utility of the method for implementation in regulatory and food laboratories was demonstrated by its application to the analysis of NMC insecticides in commercial pork tissues. In all cases, NMC residues were not present at concentrations above the LOQ determined for each type of pork tissue.

ACS Style

João F. Sousa; João N. Barros; Paulo Fernandes; Rosa Perestrelo; José S. Câmara. Simultaneous determination of N-methyl carbamate residues in pork tissues based on ultrasound assisted QuEChERS-dSPE extraction followed by reversed phase LC-FLD analysis. LWT 2021, 144, 111199 .

AMA Style

João F. Sousa, João N. Barros, Paulo Fernandes, Rosa Perestrelo, José S. Câmara. Simultaneous determination of N-methyl carbamate residues in pork tissues based on ultrasound assisted QuEChERS-dSPE extraction followed by reversed phase LC-FLD analysis. LWT. 2021; 144 ():111199.

Chicago/Turabian Style

João F. Sousa; João N. Barros; Paulo Fernandes; Rosa Perestrelo; José S. Câmara. 2021. "Simultaneous determination of N-methyl carbamate residues in pork tissues based on ultrasound assisted QuEChERS-dSPE extraction followed by reversed phase LC-FLD analysis." LWT 144, no. : 111199.

Journal article
Published: 27 February 2021 in Metabolites
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The innovation of the new psychoactive substances (NPS) market requires the rapid identification of new substances that can be a risk to public health, in order to reduce the damage from their use. Twelve seized products suspected to contain illicit substances were analyzed by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), gas chromatography coupled to mass spectrometry (GC-MS), and nuclear magnetic resonance spectroscopy (NMR). Synthetic cathinones (SCat) were found in all products, either as a single component or in mixtures. Infrared spectra of all products were consistent with the molecular structure of SCat, showing an intense absorption band at 1700–1674 cm−1, corresponding to the carbonyl stretching, a medium/strong peak at 1605–1580 cm−1, indicating stretching vibrations in the aromatic ring (C=C) and bands with relative low intensity at frequencies near 2700–2400 cm−1, corresponding to an amine salt. It was possible to identify a total of eight cathinone derivatives by GC-MS and NMR analysis: 4′-methyl-α-pyrrolidinohexanophenone (MPHP), α-pyrrolidinohexanophenone (α-PHP), 3-fluoromethcathinone (3-FMC), methedrone, methylone, buphedrone, N-ethylcathinone, and pentedrone. Among the adulterants found in these samples, caffeine was the most frequently detected substance, followed by ethylphenidate. These results highlight the prevalence of SCat in seized materials of the Portuguese market. Reference standards are usually required for confirmation, but when reference materials are not available, the combination of complementary techniques is fundamental for a rapid and an unequivocal identification of such substances.

ACS Style

João Gonçalves; Vera Alves; Joselin Aguiar; Maria Caldeira; Helena Teixeira; José Câmara. Structure Assignment of Seized Products Containing Cathinone Derivatives Using High Resolution Analytical Techniques. Metabolites 2021, 11, 144 .

AMA Style

João Gonçalves, Vera Alves, Joselin Aguiar, Maria Caldeira, Helena Teixeira, José Câmara. Structure Assignment of Seized Products Containing Cathinone Derivatives Using High Resolution Analytical Techniques. Metabolites. 2021; 11 (3):144.

Chicago/Turabian Style

João Gonçalves; Vera Alves; Joselin Aguiar; Maria Caldeira; Helena Teixeira; José Câmara. 2021. "Structure Assignment of Seized Products Containing Cathinone Derivatives Using High Resolution Analytical Techniques." Metabolites 11, no. 3: 144.

Journal article
Published: 27 February 2021 in Applied Sciences
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Phthalates are multifunctional synthetic chemicals found in a wide array of consumer and industrial products, mainly used to improve the mechanical properties of plastics, giving them flexibility and softness. In the European Union, phthalates are prohibited at levels greater than 0.1% by weight in most food packaging. In the current study, headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) was optimized, through the multivariate optimization process, and validated to evaluate the occurrence of four common phthalates, di-iso-butyl phthalate (DIBP), butyl-benzyl phthalate (BBP), di-n-octyl phthalate (DOP), and 2,2,4,4-tetrabromodiphenyl (BDE), in different food packaging. The best extraction efficiency was achieved using the polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber at 80 °C for 30 min. The validated method showed good linearity, precision (RSD < 13%), and recoveries (90.2 to 111%). The limit of detection (LOD) and of quantification (LOQ) ranged from 0.03 to 0.08 µg/L and from 0.10 to 0.24 µg/L, respectively. On average, the phthalates concentration varied largely among the assayed food packaging. DIBP was the most predominant phthalate in terms of occurrence (71.4% of analyzed simples) and concentration (from 3.61 to 10.7 μg/L). BBP was quantified in only one sample and BDE was detected in trace amounts (

ACS Style

Rosa Perestrelo; Catarina Silva; Manuel Algarra; José Câmara. Evaluation of the Occurrence of Phthalates in Plastic Materials Used in Food Packaging. Applied Sciences 2021, 11, 2130 .

AMA Style

Rosa Perestrelo, Catarina Silva, Manuel Algarra, José Câmara. Evaluation of the Occurrence of Phthalates in Plastic Materials Used in Food Packaging. Applied Sciences. 2021; 11 (5):2130.

Chicago/Turabian Style

Rosa Perestrelo; Catarina Silva; Manuel Algarra; José Câmara. 2021. "Evaluation of the Occurrence of Phthalates in Plastic Materials Used in Food Packaging." Applied Sciences 11, no. 5: 2130.

Research paper
Published: 11 February 2021 in Analytical and Bioanalytical Chemistry
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The popularity of new psychoactive substances among drug users has become a public health concern worldwide. Among them, synthetic cannabinoids (SCs) represent the largest, most diversified and fastest growing group. Commonly known as ‘synthetic marijuana’ as an alternative to cannabis, these synthetic compounds are easily accessible via the internet and are sold as ‘herbal incenses’ under different brand names with no information about the chemical composition. In the present work, we aim to integrate gas chromatography-tandem mass spectrometry (GC-MS) and nuclear magnetic resonance (NMR) data as useful strategy for the identification and confirmation of synthetic cannabinoids present in nine seized herbal incenses. The analysis of all samples allowed the initial identification of 9 SCs, namely 5 napthoylindoles (JWH-018, JWH-073, JWH-122, JWH-210, MAM-2201), APINACA, XLR-11 and CP47,497-C8 and its enantiomer. JWH-018 was the most frequently detected synthetic compound (8 of 9 samples), while APINACA and XLR-11 were only identified in one herbal product. Other non-cannabinoid drugs, including oleamide, vitamin E and vitamin E acetate, have also been detected. Oleamide and vitamin E are two adulterants, frequently added to herbal products to mask the active ingredients or added as preservatives. However, to our knowledge, no analytical data about vitamin E acetate was reported in herbal products, being the first time that this compound is identified on this type of samples. The integration data obtained from the used analytical technologies proved to be useful, allowing the preliminary identification of the different SCs in the mixture. Furthermore, the examination of mass spectral fragment ions, as well as the results of both 1D and 2D NMR experiments, enabled the identification and confirmation of the molecular structure of SCs.

ACS Style

Vera L. Alves; João L. Gonçalves; Joselin Aguiar; Maria J. Caldeira; Helena M. Teixeira; José S. Câmara. Highly sensitive screening and analytical characterization of synthetic cannabinoids in nine different herbal mixtures. Analytical and Bioanalytical Chemistry 2021, 413, 2257 -2273.

AMA Style

Vera L. Alves, João L. Gonçalves, Joselin Aguiar, Maria J. Caldeira, Helena M. Teixeira, José S. Câmara. Highly sensitive screening and analytical characterization of synthetic cannabinoids in nine different herbal mixtures. Analytical and Bioanalytical Chemistry. 2021; 413 (8):2257-2273.

Chicago/Turabian Style

Vera L. Alves; João L. Gonçalves; Joselin Aguiar; Maria J. Caldeira; Helena M. Teixeira; José S. Câmara. 2021. "Highly sensitive screening and analytical characterization of synthetic cannabinoids in nine different herbal mixtures." Analytical and Bioanalytical Chemistry 413, no. 8: 2257-2273.

Preprint
Published: 02 February 2021
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The innovation of the new psychoactive substances (NPS) market requires the rapid identification of new substances that can be a risk to public health, in order to reduce the damage due to their use. Twelve seized products suspected to contain illicit substances were analyzed by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), gas chromatography coupled to mass spectrometry (GC-MS), and nuclear magnetic resonance spectroscopy (NMR). Synthetic cathinones (SCat) were found in all products, either as a single component or in mixtures. Infrared spectra of all products were consistent with the molecular structure of SCat, showing an intense absorption band at 1700–1674 cm‐1, corresponding to the carbonyl stretching, a medium/strong peak at 1605-1580 cm-1, indicating stretching vibrations in the aromatic ring (C=C) and bands with relative low intensity at frequencies near 2700–2400 cm-1, corresponding to an amine salt. It was possible to identify a total of eight cathinone derivatives by GC-MS and NMR analysis: 4’-methyl-α-pyrrolidinohexanophenone (MPHP), α-pyrrolidinohexanophenone (α-PHP), 3-fluoromethcathinone (3-FMC), methedrone, methylone, buphedrone, N-ethylcathinone, and pentedrone. Among the adulterants found in these samples, caffeine was the most frequently detected substance, followed by ethylphenidate. These results highlight the prevalence of SCat in seized materials of the Portuguese market. Reference standards are usually required for confirmation, but when reference materials are not available, the combination of complementary techniques is fundamental for a rapid and an unequivocal identification of such substances.

ACS Style

João Gonçalves; Vera L. Alves; Joselin Aguiar; Maria Caldeira; Helena Teixeira; José S. Câmara. Metabolite Structure Assignment of Seized Products Containing Cathinone Derivatives through High Resolution Analytical Techniques. 2021, 1 .

AMA Style

João Gonçalves, Vera L. Alves, Joselin Aguiar, Maria Caldeira, Helena Teixeira, José S. Câmara. Metabolite Structure Assignment of Seized Products Containing Cathinone Derivatives through High Resolution Analytical Techniques. . 2021; ():1.

Chicago/Turabian Style

João Gonçalves; Vera L. Alves; Joselin Aguiar; Maria Caldeira; Helena Teixeira; José S. Câmara. 2021. "Metabolite Structure Assignment of Seized Products Containing Cathinone Derivatives through High Resolution Analytical Techniques." , no. : 1.

Review
Published: 24 December 2020 in Foods
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Experimental studies have provided convincing evidence that food bioactive compounds (FBCs) have a positive biological impact on human health, exerting protective effects against non-communicable diseases (NCD) including cancer and cardiovascular (CVDs), metabolic, and neurodegenerative disorders (NDDs). These benefits have been associated with the presence of secondary metabolites, namely polyphenols, glucosinolates, carotenoids, terpenoids, alkaloids, saponins, vitamins, and fibres, among others, derived from their antioxidant, antiatherogenic, anti-inflammatory, antimicrobial, antithrombotic, cardioprotective, and vasodilator properties. Polyphenols as one of the most abundant classes of bioactive compounds present in plant-based foods emerge as a promising approach for the development of efficacious preventive agents against NCDs with reduced side effects. The aim of this review is to present comprehensive and deep insights into the potential of polyphenols, from their chemical structure classification and biosynthesis to preventive effects on NCDs, namely cancer, CVDs, and NDDS. The challenge of polyphenols bioavailability and bioaccessibility will be explored in addition to useful industrial and environmental applications. Advanced and emerging extraction techniques will be highlighted and the high-resolution analytical techniques used for FBCs characterization, identification, and quantification will be considered.

ACS Style

José S. Câmara; Bianca R. Albuquerque; Joselin Aguiar; Rúbia C. G. Corrêa; João L. Gonçalves; Daniel Granato; Jorge A. M. Pereira; Lillian Barros; Isabel C. F. R. Ferreira. Food Bioactive Compounds and Emerging Techniques for Their Extraction: Polyphenols as a Case Study. Foods 2020, 10, 37 .

AMA Style

José S. Câmara, Bianca R. Albuquerque, Joselin Aguiar, Rúbia C. G. Corrêa, João L. Gonçalves, Daniel Granato, Jorge A. M. Pereira, Lillian Barros, Isabel C. F. R. Ferreira. Food Bioactive Compounds and Emerging Techniques for Their Extraction: Polyphenols as a Case Study. Foods. 2020; 10 (1):37.

Chicago/Turabian Style

José S. Câmara; Bianca R. Albuquerque; Joselin Aguiar; Rúbia C. G. Corrêa; João L. Gonçalves; Daniel Granato; Jorge A. M. Pereira; Lillian Barros; Isabel C. F. R. Ferreira. 2020. "Food Bioactive Compounds and Emerging Techniques for Their Extraction: Polyphenols as a Case Study." Foods 10, no. 1: 37.

Journal article
Published: 24 December 2020 in LWT
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Food deterioration caused by microbial agents often involve the formation of biogenic amines (BAs), which can have harmful effects on human health. In this study a set of BAs - tryptamine, cadaverine, putrescine, spermine, histamine, tyramine, and spermidine, were simultaneously analysed to monitor their occurrence in different types of tuna samples. An improved extraction approach involving ultrasound-assisted microextraction (USAμET) followed by derivatization with dansyl chloride (DnsCl) and analysis by ultrahigh performance liquid chromatography (UHPLC) with fluorescence detection was validated for BAs quantification. The performance of the USAμET/UHPLC-FLR was assessed by studying the limits of detection (LOD) and quantification (LOQ), linear dynamic range (LDR), precision (intra and inter-day) and matrix effect (ME). Good linearity (r2>0.98), LODs (from 0.98 to 8.57 mg kg-1) and LOQs (3.20 to 25.6 mg kg-1) were achieved for all BAs analysed. Recoveries ranged from 76 % to 106 %, with relative standard deviations (RSD) lower than 5.0 %. ME was determined from 7.52 to 50 % and the intra and inter-day precisions ranged from 4.7 to 11.6 % and 5.5 to 14.2%, respectively. BAs levels varied significantly from 4.09±0.8 mg kg-1 of putrescine in olive oil canned samples to 577.9±5.9 mg kg-1 of cadaverine in natural canned samples. Tryptamine and tyramine were not detected in any of the samples analysed, while spermine and spermidine were found in 85.7 % of the assayed tuna samples. Cadaverine was the most dominant BA with concentrations ranging from 54.3±2.5 mg kg-1, in olive oil canned tuna, to 577.9±5.9 mg kg-1, in natural canned samples, whereas putrescine had the lowest concentration (average 6.9±2.5 mg kg-1). The validated methodology revealed important improvements in terms of simplification of the experimental layout, expressed in the low sample and reagent amounts, in addition to less time-consuming and labour-intensive requirements that did not compromise the analytical performance.

ACS Style

Joanna K.G. Pataca; Priscilla Porto-Figueira; Jorge A.M. Pereira; Helena Caldeira; José S. Câmara. Profiling the occurrence of biogenic amines in different types of tuna samples using an improved analytical approach. LWT 2020, 139, 110804 .

AMA Style

Joanna K.G. Pataca, Priscilla Porto-Figueira, Jorge A.M. Pereira, Helena Caldeira, José S. Câmara. Profiling the occurrence of biogenic amines in different types of tuna samples using an improved analytical approach. LWT. 2020; 139 ():110804.

Chicago/Turabian Style

Joanna K.G. Pataca; Priscilla Porto-Figueira; Jorge A.M. Pereira; Helena Caldeira; José S. Câmara. 2020. "Profiling the occurrence of biogenic amines in different types of tuna samples using an improved analytical approach." LWT 139, no. : 110804.

Journal article
Published: 09 December 2020 in Foods
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Aroma is a crucial criterion to assess the quality of apple fruits, juices, and ciders. The aim of this study was to explore similarities and differences in volatile profiles among apple fruits, juices, and ciders from different apple varieties (Festa, Branco, and Domingos) by headspace solid-phase microextraction gas chromatography–mass spectroscopy (HS–SPME/GC–MS). A total of 142 volatile organic compounds (VOCs) were identified, but only 9 were common in all analysed matrices and apple-tested varieties. Esters, alcohols, and aldehydes presented a higher concentration in apple fruits and juices, whereas esters, alcohols, and acids were dominant in ciders. Moreover, there were unique VOCs for each matrix and for each variety, highlighting the importance of the selection of apple varieties as an important factor to obtain good sensory and quality ciders, multiple benefits, and legal protection against the misuse of local products.

ACS Style

Sonia Medina; Rosa Perestrelo; Regina Pereira; José S. Câmara. Evaluation of Volatilomic Fingerprint from Apple Fruits to Ciders: A Useful Tool to Find Putative Biomarkers for Each Apple Variety. Foods 2020, 9, 1830 .

AMA Style

Sonia Medina, Rosa Perestrelo, Regina Pereira, José S. Câmara. Evaluation of Volatilomic Fingerprint from Apple Fruits to Ciders: A Useful Tool to Find Putative Biomarkers for Each Apple Variety. Foods. 2020; 9 (12):1830.

Chicago/Turabian Style

Sonia Medina; Rosa Perestrelo; Regina Pereira; José S. Câmara. 2020. "Evaluation of Volatilomic Fingerprint from Apple Fruits to Ciders: A Useful Tool to Find Putative Biomarkers for Each Apple Variety." Foods 9, no. 12: 1830.