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Terpenoids are a large class of natural secondary plant metabolites which are highly diverse in structure, formed from isoprene units (C-5), associated with a wide range of biological properties, including antioxidant, antimicrobial, anti-inflammatory, antiallergic, anticancer, antimetastatic, antiangiogenesis, and apoptosis induction, and are considered for potential application in the food, cosmetics, pharmaceutical, and medical industries. In plants, terpenoids exert a variety of basic functions in growth and development. This review gives an overview, highlighting the current knowledge of terpenoids and recent advances in our understanding of the organization, regulation, and diversification of core and specialized terpenoid metabolic pathways and addressing the most important functions of volatile and non-volatile specialized terpenoid metabolites in plants. A comprehensive description of different aspects of plant-derived terpenoids as a sustainable source of bioactive compounds, their biosynthetic pathway, the several biological properties attributed to these secondary metabolites associated with health-promoting effects, and their potential industrial applications in several fields will be provided, and emerging and green extraction methods will also be discussed. In addition, future research perspectives within this framework will be highlighted. Literature selection was carried out using the National Library of Medicine, PubMed, and international reference data for the period from 2010 to 2024 using the keyword “terpenoids”. A total of 177,633 published papers were found, of which 196 original and review papers were included in this review according to the criteria of their scientific reliability, their completeness, and their relevance to the theme considered.

Neurodegenerative disorders (NDDs) such as Alzheimer’s (AD) and Parkinson’s (PD) are on the rise, robbing people of their memories and independence. While risk factors such as age and genetics play an important role, exciting studies suggest that a diet rich in foods from plant origin may offer a line of defense. These kinds of foods, namely fruits and vegetables, are packed with a plethora of powerful bioactive secondary metabolites (SBMs), including terpenoids, polyphenols, glucosinolates, phytosterols and capsaicinoids, which exhibit a wide range of biological activities including antioxidant, antidiabetic, antihypertensive, anti-Alzheimer’s, antiproliferative, and antimicrobial properties, associated with preventive effects in the development of chronic diseases mediated by oxidative stress such as type 2 diabetes mellitus, respiratory diseases, cancer, cardiovascular diseases, and NDDs. This review explores the potential of SBMs as theravention agents (metabolites with therapeutic and preventive action) against NDDs. By understanding the science behind plant-based prevention, we may be able to develop new strategies to promote brain health and prevent the rise in NDDs. The proposed review stands out by emphasizing the integration of multiple SBMs in plant-based foods and their potential in preventing NDDs. Previous research has often focused on individual compounds or specific foods, but this review aims to present a comprehensive fingerprint of how a diet rich in various SBMs can synergistically contribute to brain health. The risk factors related to NDD development and the diagnostic process, in addition to some examples of food-related products and medicinal plants that significantly reduce the inhibition of acetylcholinesterase (AChE), butyrylcholinesterase (BChE), and β-site amyloid precursor protein (APP) cleaving enzyme 1 (BACE1), are highlighted.

Growing consumer demand for environmentally conscious, sustainable, and helpful products has prompted scientists and industry experts worldwide to look for inventive approaches to mitigate the environmental impact, particularly concerning agricultural and industrial waste. Among the by-products of winemaking, grape pomace (skins, seeds, stems) has the potential to be economically valuable as it is rich in value-added compounds (e.g., phenolic compounds, fibers, flavonoids, anthocyanins, terpenoids) related to health (e.g., antioxidant, antimicrobial, anti-inflammatory, cardioprotective effects) and technological issues (e.g., extraction of value-added compounds). These value-added compounds can be extracted using emerging green extraction techniques and then used in the food industry as preservatives, colorants, and for the formulation of functional foods, as well as in the development of smart food packaging. This review provides an overview of the value-added compounds identified in grape pomace, the emerging green extraction, and integrated approaches to extract value-added compounds based on the literature published in the last five years. The potential applications of these value-added compounds have been extensively researched for the food industry.

Prostate cancer (PCa) continues to be the second most common malignant tumour and the main cause of oncological death in men. Investigating endogenous volatile organic metabolites (VOMs) produced by various metabolic pathways is emerging as a novel, effective, and non-invasive source of information to establish the volatilomic biosignature of PCa. In this study, headspace solid-phase microextraction combined with gas chromatography–mass spectrometry (HS-SPME/GC-MS) was used to establish the urine volatilomic profile of PCa and identify VOMs that can discriminate between the two investigated groups. This non-invasive approach was applied to oncological patients (PCa group, n = 26) and cancer-free individuals (control group, n = 30), retrieving a total of 147 VOMs from various chemical families. This included terpenes, norisoprenoid, sesquiterpenes, phenolic, sulphur and furanic compounds, ketones, alcohols, esters, aldehydes, carboxylic acid, benzene and naphthalene derivatives, hydrocarbons, and heterocyclic hydrocarbons. The data matrix was subjected to multivariate analysis, namely partial least-squares discriminant analysis (PLS-DA). Accordingly, this analysis showed that the group under study presented different volatomic profiles and suggested potential PCa biomarkers. Nevertheless, a larger cohort of samples is required to boost the predictability and accuracy of the statistical models developed.

Designing and manufacturing functional bioactive ingredients and pharmaceuticals have grown worldwide. Consumers demand for safe ingredients and concerns over harmful synthetic additives have prompted food manufacturers to seek safer and sustainable alternative solutions. In recent years the preference by consumers to natural bioactive agents over synthetic compounds increased exponentially, and consequently, naturally derived phytochemicals and bioactive compounds, with antimicrobial and antioxidant properties, becoming essential in food packaging field. In response to societal needs, packaging needs to be developed based on sustainable manufacturing practices, marketing strategies, consumer behaviour, environmental concerns, and the emergence of new technologies, particularly bio- and nanotechnology. This critical systematic review assessed the role of antioxidant and antimicrobial compounds from natural resources in food packaging and consumer behaviour patterns in relation to phytochemical and biologically active substances used in the development of food packaging. The use of phytochemicals and bioactive compounds inside packaging materials used in food industry could generate unpleasant odours derived from the diffusion of the most volatile compounds from the packaging material to the food and food environment. These consumer concerns must be addressed to understand minimum concentrations that will not affect consumer sensory and aroma negative perceptions. The research articles were carefully chosen and selected by following the Preferred Reporting Items for Systematic Reviews (PRISMA) guidelines.

Prostate cancer (PCa) is the most frequently occurring type of malignant tumor and a leading cause of oncological death in men. PCa is very heterogeneous in terms of grade, phenotypes, and genetics, displaying complex features. This tumor often has indolent growth, not compromising the patient’s quality of life, while its more aggressive forms can manifest rapid growth with progression to adjacent organs and spread to lymph nodes and bones. Nevertheless, the overtreatment of PCa patients leads to important physical, mental, and economic burdens, which can be avoided with careful monitoring. Early detection, even in the cases of locally advanced and metastatic tumors, provides a higher chance of cure, and patients can thus go through less aggressive treatments with fewer side effects. Furthermore, it is important to offer knowledge about how modifiable risk factors can be an effective method for reducing cancer risk. Innovations in PCa diagnostics and therapy are still required to overcome some of the limitations of the current screening techniques, in terms of specificity and sensitivity. In this context, this review provides a brief overview of PCa statistics, reporting its incidence and mortality rates worldwide, risk factors, and emerging screening strategies.

Entomotherapy, the use of insects for medicinal purposes, has been practised for centuries in many countries around the world. More than 2100 edible insect species are eaten by humans, but little is known about the possibility of using these insects as a promising alternative to traditional pharmaceuticals for treating diseases. This review offers a fundamental understanding of the therapeutic applications of insects and how they might be used in medicine. In this review, 235 insect species from 15 orders are reported to be used as medicine. Hymenoptera contains the largest medicinal insect species, followed by Coleoptera, Orthoptera, Lepidoptera, and Blattodea. Scientists have examined and validated the potential uses of insects along with their products and by-products in treating various diseases, and records show that they are primarily used to treat digestive and skin disorders. Insects are known to be rich sources of bioactive compounds, explaining their therapeutic features such as anti-inflammatory, antimicrobial, antiviral, and so on. Challenges associated with the consumption of insects (entomophagy) and their therapeutic uses include regulation barriers and consumer acceptance. Moreover, the overexploitation of medicinal insects in their natural habitat has led to a population crisis, thus necessitating the investigation and development of their mass-rearing procedure. Lastly, this review suggests potential directions for developing insects used in medicine and offers advice for scientists interested in entomotherapy. In future, entomotherapy may become a sustainable and cost-effective solution for treating various ailments and has the potential to revolutionize modern medicine.

Consumers in developed and Western European countries are becoming more aware of the impact of food on their health, and they demand clear, transparent, and reliable information from the food industry about the products they consume. They recognise that food safety risks are often due to the unexpected presence of contaminants throughout the food supply chain. Among these, mycotoxins produced by food-infecting fungi, endogenous toxins from certain plants and organisms, pesticides, and other drugs used excessively during farming and food production, which lead to their contamination and accumulation in foodstuffs, are the main causes of concern. In this context, the goals of this review are to provide a comprehensive overview of the presence of toxic molecules reported in foodstuffs since 2020 through the Rapid Alert System for Food and Feed (RASFF) portal and use chromatography to address this challenge. Overall, natural toxins, environmental pollutants, and food-processing contaminants are the most frequently reported toxic molecules, and liquid chromatography and gas chromatography are the most reliable approaches for their control. However, faster, simpler, and more powerful analytical procedures are necessary to cope with the growing pressures on the food chain supply.

Cancer remains the second most common cause of death after cardiovascular diseases, accounting for nearly 10 million deaths in 2020. Although the incidence of cancer increases considerably with age, the cancer burden can also be reduced and have a high chance of cure through early detection, appropriate treatment, and care of patients. The development of high-throughput analytical approaches, like matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS), contributes to identifying a pool of proteins/peptides as putative biomarkers for the early detection, diagnosis, and tumor progression. The purpose of the current review is to present an updated outline of recent proteome/peptidome research to establish putative cancer biomarkers using MALDI-TOF MS and highlight the applicability of statistical analysis in the oncology field. The pros and cons of MALDI-TOF MS application on cancer diagnostics and monitoring will be discussed, as well as compared with tandem mass spectrometry (MS/MS)-based proteomics (e.g., liquid chromatography–tandem mass spectrometry). In addition, pre-analytical (e.g., sample quality control) and analytical (e.g., sample pre-treatment, instrumental analytical conditions) properties that influence the robustness of MALDI-TOF MS data will be also discussed.

The huge amount of grape pomace (GP) generated every year worldwide, particularly in Europe, creates negative impacts at the economic and environmental levels. As far as we know, scarce research has been done on the volatilomic fingerprint of GP. To meet consumer demand for healthy foods, there is a growing interest in the characterization of particular volatile organic metabolites (VOMS) in GP that can be used for industrial applications, including the food industry. In this study, the volatilomic fingerprint of GP obtained from different Vitis vinifera L. grapes was established by solid phase microextraction (HS-SPME) combined to gas chromatography-mass spectrometry (GC-MS), to explore the properties of most dominant VOMs in a context of its application on marketable products. A total of 52 VOMs belonging to different chemical families were identified. Alcohols, carbonyl compounds, and esters, are the most dominant, representing 38.8, 29.3, and 24.2% of the total volatile profile of the investigated GP, respectively. Esters (e.g., isoamyl acetate, hexyl acetate, ethyl hexanoate) and alcohols (e.g., 3-methyl butan-2-ol, hexan-1-ol) can be used as flavoring agents with potential use in the food industry, and in the cosmetic industry, for fragrances production. In addition, the identified terpenoids (e.g., menthol, ylangene, limonene) exhibit antioxidant, antimicrobial, and anticancer, biological properties, among others, boosting their potential application in the pharmaceutical industry. The obtained results revealed the potential of some VOMs from GP to replace synthetic antioxidants, colorants, and antimicrobials used in the food industry, and in the cosmetic and pharmaceutical industry, meeting the increasing consumer demand for natural alternative compounds.

The fortified wines that originated in Mediterranean countries have, in common, a high alcohol content to increase their shelf-life during long journeys to northern Europe and the American continent. Nowadays, the world’s better-known wines, including Marsala, Madeira, Port, and Sherry, due to their high alcoholic content, sweet taste, and intense aromatic profile, are designated as dessert wines and sometimes served as aperitifs. This review gives an overview of the traditional vinification process, including the microbiota and autochthonous yeast, as well as the regulatory aspects of the main Italian, Portuguese, and Spanish fortified wines. The winemaking process is essential to defining the volatile organic compounds (VOCs) that characterize the aroma of each fortified wine, giving them an organoleptic fingerprint and “terroir” characteristics. The various volatile and odorous compounds found in fortified wines during the oxidative aging are discussed in the last part of this review.

The increasing demand for food to feed an exponentially growing population, the fast evolution of climate changes, how global warming affects soil productivity, and the erosion of arable lands, create enormous pressure on the food chain. This problem is particularly evident for fresh fruits and vegetables that have a short shelf life. For this reason, food safety precautions are not always a priority and they are often overused to increase the productivity and shelf life of these food commodities, causing concerns among consumers and public authorities. In this context, this review discusses the potential of microextraction in comparison to conventional extraction approaches as a strategy to improve the survey of food safety requirements. Accordingly, selected examples reported in the literature in the last five years will focus on the detection and quantification of pesticides, antibiotics, hormones, and preservatives in fresh fruits and vegetables using different extraction approaches. Overall, the use of microextraction techniques to survey the presence of contaminants in the food chain is very advantageous, involving simpler and faster protocols, reduced amounts of solvents and samples, and consequently, reduced waste produced during analysis while conserving a high potential for automation. Additionally, this higher greener profile of the microextraction techniques will boost a progressive substitution of conventional extraction approaches by microextraction processes in most analytical applications, including the survey of food chain safety.

Atropine and scopolamine belong to the tropane alkaloid (TA) family of natural toxins. They can contaminate teas and herbal teas and appear in infusions. Therefore, this study focused on analyzing atropine and scopolamine in 33 samples of tea and herbal tea infusions purchased in Spain and Portugal to determine the presence of these compounds in infusions brewed at 97 °C for 5 min. A rapid microextraction technique (µSPEed®) followed by high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) was used to analyze the selected TAs. The results showed that 64% of the analyzed samples were contaminated by one or both toxins. White and green teas were generally more contaminated than black and other herbal teas. Of the 21 contaminated samples, 15 had concentrations above the maximum limit for liquid herbal infusions (0.2 ng/mL) set by Commission Regulation (EU) 2021/1408. In addition, the effects of heating conditions (time and temperature) on atropine and scopolamine standards and naturally contaminated samples of white, green, and black teas were evaluated. The results showed that at the concentrations studied (0.2 and 4 ng/mL), there was no degradation in the standard solutions. Brewing with boiling water (decoction) for 5 and 10 min allowed for higher extraction of TAs from dry tea to infusion water.

The aim of the current study was to provide a useful platform to identify characteristic molecular markers related to the authenticity of Italian fortified wines. For this purpose, the volatilomic fingerprint of the most popular Italian fortified wines was established using headspace solid-phase microextraction combined with gas chromatography–mass spectrometry (HS-SPME/GC-MS). Several volatile organic compounds (VOCs), belonging with distinct chemical groups, were identified, ten of which are common to all the analyzed fortified Italian wines. Terpenoids were the most abundant chemical group in Campari bitter wines due to limonene’s high contribution to the total volatilomic fingerprint, whereas for Marsala wines, alcohols and esters were the most predominant chemical groups. The fortified Italian wines VOCs network demonstrated that the furanic compounds 2-furfural, ethyl furoate, and 5-methyl-2-furfural, constitute potential molecular markers of Marsala wines, while the terpenoids nerol, α-terpeniol, limonene, and menthone isomers, are characteristic of Vermouth wines. In addition, butanediol was detected only in Barolo wines, and β-phellandrene and β-myrcene only in Campari wines. The obtained data reveal an adequate tool to establish the authenticity and genuineness of Italian fortified wines, and at the same time constitute a valuable contribution to identify potential cases of fraud or adulteration to which they are subject, due to the high commercial value associated with these wines. In addition, they contribute to the deepening of scientific knowledge that supports its valorization and guarantee of quality and safety for consumers.

The overuse of antibiotics in the healthcare, veterinary, and agricultural industries has led to the development of antimicrobial resistance (AMR), resulting in significant economic losses worldwide and a growing healthcare problem that urgently needs to be solved. Plants produce a variety of secondary metabolites, making them an area of interest in the search for new phytochemicals to cope with AMR. A great part of agri-food waste is of plant origin, constituting a promising source of valuable compounds with different bioactivities, including those against antimicrobial resistance. Many types of phytochemicals, such as carotenoids, tocopherols, glucosinolates, and phenolic compounds, are widely present in plant by-products, such as citrus peels, tomato waste, and wine pomace. Unveiling these and other bioactive compounds is therefore very relevant and could be an important and sustainable form of agri-food waste valorisation, adding profit for local economies and mitigating the negative impact of these wastes’ decomposition on the environment. This review will focus on the potential of agri-food waste from a plant origin as a source of phytochemicals with antibacterial activity for global health benefits against AMR.

The potential development of a rapid and highly sensitive breast cancer (BC) diagnostic method has been increasingly investigated by many researchers in order to significantly improve the diagnosis of this disease that affects millions of women worldwide. Thus, this investigation aimed to establish a potential BC urinary peptidomic pattern using one-dimensional sodium dodecyl sulfate-polyacrylamide gel electrophoresis (1D SDS-PAGE) coupled with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) as a useful approach for BC diagnosis. The results of Lowry’s assay demonstrated that the total protein concentration increased after precipitation and that the healthy control group (HCs, 160 to 318 µg/mL, 142 ± DD µg/mL, on average) presented higher total protein content than the BC patients (140 to 311 µg/mL, 115 ± DD µg/mL, on average). Related to MALDI-TOF MS analysis, the results revealed that four peptide ion biosignatures (m/z 1046.5, 1062.5, 1237.7 and 1727.9) allowed the discrimination between BC patients and HCs. The distinction efficiency and accuracy of BC urine peptides were determined by receiver operating characteristic (ROC) curve analysis that enabled the recognition of some features with great sensitivity (88%) and specificity (98%). Therefore, the obtained data revealed MALDI-TOF MS as a powerful tool to explore peptidomic biosignatures due to its speed, sensitivity, and mass accuracy, which allow the establishment of novel disease biomarkers.

Aroma compounds play a key role in wine quality due to their importance in wine aroma. The aim of the present study is to investigate the influence of cold pre-fermentative maceration (CPM) treatment on aromatic and sensory properties of white wines from four grape varieties (Tempranillo Blanco, Maturana Blanca, Viura and Garnacha Blanca) during two consecutive years (2019 and 2020). A total of 62 aroma compounds belonging to different chemical families were identified using headspace solid-phase microextraction combined with gas chromatography mass spectrometry (HS-SPME/GC-MS). CPM treatment enhanced the total relative concentration of alcohols, esters and acids compared to control wines. Regarding sensorial properties, esters made the greatest contribution to the studied white wines, mainly through the development of floral and fruity notes. On the other hand, CPM treatment did not significantly influence the total relative concentration of terpenoids, and different trends were observed according to grape variety and vintage. The obtained results showed differences in the wine’s aromatic complexity according to the grape variety, the vintage and the treatment applied and suggested that CPM treatment could represent a suitable approach to manipulate the aromatic profile and enhance the aromatic quality and complexity of wine.

Patulin (PAT) is a mycotoxin produced in fruits, especially in apples, by diverse fungal species that can be transferred into industrial apple juice during processing. An accurate, effective, and selective method has been validated for the quantification of PAT in different commercial apple juices by combining a modified µ-QuEChERS procedure with high-pressure liquid chromatography (LC) equipped with a triple quadrupole mass spectrometer (QqQMS). This sample extraction procedure reduced interference from the sugar-rich matrix, and the separation was performed using the C18 Atlantis T3 column within 10 min. PAT was found by MS with electrospray negative ionization (ESI−) in the mode of multiple reaction monitoring (MRM). The correlation coefficient (R2 = 0.999) satisfied the prerequisite of linearity for PAT in the concentration range of 2–50 μg/kg. The limits of detection (LOD) and quantification (LOQ) of PAT were 0.32 and 1.15 μg/kg, respectively, which were compliant with the maximum levels settled in Commission Regulation (EC) No. 1881/2006. The recoveries were within the 92–103% range, at three fortified levels of 2, 20 and 50 μg/kg, with relative standard deviations lower than 7%. Based on analytical validation, it was confirmed that the µ-QuEChERS/HPLC-MS/MS method is an enhanced, reliable, and quick approach for determination of PAT in apple juice. The current approach proposes reduced sample preparation and analysis time. In addition, it is economical, environmentally friendly, and simpler to implement in comparison to traditional approaches.

For a long time, the importance of sample preparation and extraction in the analytical performance of the most diverse methodologies have been neglected. Cumbersome techniques, involving high sample and solvent volumes have been gradually miniaturized from solid-phase and liquid-liquid extractions formats and microextractions approaches are becoming the standard in different fields of research. In this context, this review is devoted to the analysis of bioactive compounds in foods using different microextraction approaches reported in the literature since 2015. But microextraction also represents an opportunity to mitigate the environmental impact of organic solvents usage, as well as lab equipment. For this reason, in the recent literature, phenolics and alkaloids extraction from fruits, medicinal herbs, juices, and coffee using different miniaturized formats of solid-phase extraction and liquid-liquid microextraction are the most popular applications. However, more ambitious analytical limits are continuously being reported and emergent sorbents based on carbon nanotubes and magnetic nanoparticles will certainly contribute to this trend. Additionally, ionic liquids and deep eutectic solvents constitute already the most recent forefront of innovation, substituting organic solvents and further improving the current microextraction approaches.

Intoxication due to the consumption of poppy seed teas has been reported due to their contamination with opium alkaloids (OAs). In this work, an efficient methodology based on microsolid-phase extraction (µSPEed®) followed by gas chromatography–mass spectrometry (GC-MS) has been optimized to quantify five OAs in poppy seed teas. Nine cartridges (C4, C8, C18, silica, APS, PFAs, PS/DVB-RP, PS/DVB-SCX and PS/DVB-SAX), pH levels, cycles and elution solvents were evaluated. The method was validated and applied to study the transfer of OAs by evaluating water temperatures, infusion times and seed amounts. The highest transfer rates (71% for morphine, 96% for thebaine, and 100% for codeine, noscapine and papaverine) were achieved at 90°C, 5 min, with 4 g. These conditions were used to quantify the OAs in four teas prepared from different seeds. A high amount of morphine (1563 µg/L) was found in one tea, indicating that the seeds had a concentration twice the maximum limit, highlighting the need to warn the population of this dangerous practice.

It is known that many bacteria are susceptible to low pH, but it is less clear how the acid nature influences this susceptibility. The objective of this work was to evaluate the susceptibility of selected bacteria to different low pH conditions and to understand if their tolerance is affected by the type of acid (organic vs inorganic) in the media acidification. Strains of different species of human pathogenic bacteria were cultivated at different acidic conditions, using organic or inorganic acids. Overall, we verified that tolerance to acidic conditions is dependent on the type of acid used to acidify the growing medium, organic or inorganic. The strains analysed, although having different tolerance to low pH, were shown to be more susceptible to organic than inorganic acids. This result shows that beyond the pH of the media, the nature of the acid affects bacterial growth. Such a result has consequences in the evaluation of the efficiency of an antibacterial extract, which should take into consideration the differential susceptibility of bacteria to low pHs obtained using organic or inorganic acids.

Anthocyanins are widespread and biologically active water-soluble phenolic pigments responsible for a wide range of vivid colours, from red (acidic conditions) to purplish blue (basic conditions), present in fruits, vegetables, and coloured grains. The pigments’ stability and colours are influenced mainly by pH but also by structure, temperature, and light. The colour-stabilizing mechanisms of plants are determined by inter- and intramolecular co-pigmentation and metal complexation, driven by van der Waals, π–π stacking, hydrogen bonding, and metal-ligand interactions. This group of flavonoids is well-known to have potent anti-inflammatory and antioxidant effects, which explains the biological effects associated with them. Therefore, this review provides an overview of the role of anthocyanins as natural colorants, showing they are less harmful than conventional colorants, with several technological potential applications in different industrial fields, namely in the textile and food industries, as well as in the development of photosensitizers for dye-sensitized solar cells, as new photosensitizers in photodynamic therapy, pharmaceuticals, and in the cosmetic industry, mainly on the formulation of skin care formulations, sunscreen filters, nail colorants, skin & hair cleansing products, amongst others. In addition, we will unveil some of the latest studies about the health benefits of anthocyanins, mainly focusing on the protection against the most prevalent human diseases mediated by oxidative stress, namely cardiovascular and neurodegenerative diseases, cancer, and diabetes. The contribution of anthocyanins to visual health is also very relevant and will be briefly explored.

Finger lime is receiving growing attention as an ingredient of gastronomic preparations of haute cuisine for its delicious flavor and fragrance and for its appealing aspect. Volatile compounds play a crucial role in determining the organoleptic characteristics of the fruit and its pleasantness for consumers. The aim of the present study was to investigate the volatile profiles by headspace solid phase micro-extraction (HS-SPME) coupled to gas chromatography–mass spectrometry (GC–MS) in the peel and, for the first time, in the pulp of three Australian finger lime cultivars grown in Sicily (southern Italy): Pink Pearl, Sanguinea, and Faustrime, allowing to overall identify 84 volatile organic compounds (VOCs). The analytical data showed that the three cultivars were characterized by distinct volatile chemotypes: limonene/sabinene/bicyclogermacrene in the Pink Pearl, limonene/γ-terpinene/bicyclogermacrene in the Sanguinea, and limonene/β-phellandrene/γ-terpinene in the Faustrime. Moreover, some volatiles, found exclusively in one cultivar, could be considered potential markers of the individual cultivar. PCA allowed us to clearly discriminate the samples into three clusters: the first related to the Sanguinea peel, the second to the Faustrime peel, and a third group associated with the Pink Pearl peel along with the pulp of the three cultivars. Accordingly, the VOCs that mostly contributed to the differentiation of the three finger lime cultivars were also identified. Among them, D-limonene, sabinene γ-terpinene, α-pinene, α-phellandrene, β-myrcene, p-cymene, linalool, δ-elemene, ledene, bicyclogermacrene β-citronellol, α-bergamotene, α-caryophillene, and β-bisabolene, have been previously reported to exhibit important biological activities, suggesting that these cultivars, in addition to possessing unique volatile profiles, can show promise for several applications in pharmaceutical and food industry, namely for development of functional foods.

Coffee is one of the world’s most popular beverages, and its consumption generates copious amounts of waste. The most relevant by-product of the coffee industry is the spent coffee grounds, with 6 million tons being produced worldwide per year. Although generally treated as waste, spent coffee grounds are a rich source of several bioactive compounds with applications in diverse industrial fields. The present work aimed at the analysis of spent coffee grounds from different geographical origins (Guatemala, Colombia, Brazil, Timor, and Ethiopia) for the identification of bioactive compounds with industrial interest. For this purpose, the identification and quantification of the bioactive compounds responsible for the antioxidant activity attributed to the spent coffee grounds were attempted using miniaturized solid-phase extraction (µ-SPEed), combined with ultrahigh-performance liquid chromatography with photodiode array detection (UHPLC-PDA). After validation of the µ-SPEed/UHPLC-PDA method, this allowed us to conclude that caffeine and 5-caffeoylquinic acid (5-CQA) are the most abundant bioactive compounds in all samples studied. The total phenolic content (TPC) and antioxidant activity are highest in Brazilian samples. The results obtained show that spent coffee grounds are a rich source of bioactive compounds, supporting its bioprospection based on the circular economy concept closing the loop of the coffee value chain, toward the valorization of coffee by-products.

This work presents an optimized methodology based on the miniaturization of the original QuEChERS (μ-QuEChERS) followed by liquid chromatography coupled to mass spectrometry (HPLC-MS/MS) for the determination of tropane alkaloids (TAs), atropine, and scopolamine in leafy vegetable samples. The analytical methodology was successfully validated, demonstrating quantitation limits (MQL) ≤ 2.3 ng/g, good accuracy, and precision, with recoveries between 90–100% and RSD ≤ 13% for both analytes. The method was applied to the analysis of TA-producing plants (Brugmansia versicolor, Solandra maxima, and Convolvulus arvensis). High concentrations of scopolamine were found in flowers (1771 mg/kg) and leaves (297 mg/kg) of B. versicolor. The highest concentration of atropine was found in flowers of S. maxima (10.4 mg/kg). Commercial mixed leafy vegetables contaminated with B. versicolor and S. maxima were analysed to verify the efficacy of the method, showing recoveries between 82 and 110% for both analytes. Finally, the method was applied to the analysis of eighteen samples of leafy vegetables, finding atropine in three samples of mixed leafy vegetables, with concentrations of 2.7, 3.2, and 3.4 ng/g, and in nine samples with concentrations ≤MQL. In turn, scopolamine was only found in a sample of chopped Swiss chard with a concentration ≤MQL.

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.

Volatile organic metabolites (VOMs) present in different spices can provide distinct analytical biosignatures related to organoleptic properties and health benefits. This study aimed to establish the volatilomic fingerprint of six of the most consumed spices all over the world (saffron (Crocus sativus L.), cinnamon (Cinnamomum verum), cumin (Cuminum cyminum L.), black pepper, (Piper nigrum L.), sweet paprika (Capsicum annuum L.), and curry (a mix of different herbs and spices)). Based on headspace solid phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS) analysis, this is a powerful strategy to explore and establish the spice’s volatile pattern and unravel the potential health benefits related to the most important VOMs identified in each spice. This comprehensive knowledge will help in the definition of their authenticity, while simultaneously protecting against potential frauds and adulterations. A total of 162 VOMs were identified. Semi-quantitative assessments revealed that terpenoids and sesquiterpenoids amounted to the major volatile class in the investigated spices, except for cinnamon, where carbonyl compounds are the major group. Most of the studied spices comprised key characteristics of aroma and health bioactive compounds, e.g., dihydrojuneol in saffron, cinnamaldehyde in cinnamon, cuminaldehyde in cumin and curry, and caryophyllene in black pepper. The principal component analysis (PCA) and partial least-squares discriminant analysis (PLS-DA) successfully discriminated the investigated spices, being α-cubebene, 3-methyl butanal, β-patchoulene and β-selinene, the most important VOMs (highest VIP’s) that contributed to its discrimination. Moreover, some VOMs have a high influence on the spice’s bioactive potential, helping to prevent certain diseases including cancer, inflammatory-related diseases, diabetes, and cardiovascular diseases.

Chromatography was born approximately one century ago and has undergone outstanding technological improvements in innovation, research, and development since then that has made it fundamental to advances in knowledge at different levels, with a relevant impact on the well-being and health of individuals. Chromatography boosted a comprehensive and deeper understanding of the complexity and diversity of human–environment interactions and systems, how these interactions affect our life, and the several societal challenges we are currently facing, namely those related to the sustainability of our planet and the future generations. From the life sciences, which allowed us to identify endogenous metabolites relevant to disease mechanisms, to the OMICS field, nanotechnology, clinical and forensic analysis, drug discovery, environment, and “foodprint”, among others, the wide range of applications of today’s chromatographic techniques is impressive. This is fueled by a great variability of powerful chromatographic instruments currently available, with very high sensitivity, resolution, and identification capacity, that provide a strong basis for an analytical platform able to support the challenging demands of the postgenomic and post COVID-19 eras. Within this context, this review aims to address the great utility of chromatography in helping to cope with several societal-based challenges, such as the characterization of disease and/or physiological status, and the response to current agri-food industry challenges of food safety and sustainability, or the monitoring of environmental contamination. These are increasingly important challenges considering the climate changes, the tons of food waste produced every day, and the exponential growth of the human population. In this context, the principles governing the separation mechanisms in chromatography as well the different types and chromatographic techniques will be described. In addition, the major achievements and the most important technological advances will be also highlighted. Finally, a set of studies was selected in order to evince the importance of different chromatographic analyses to understand processes or create fundamental information in the response to current societal challenges.

In recent years, the concerns and demands by consumers for the high quality and safety for natural and processed plant-based and animal foods has increased significantly [...]

Coffee is one of the most popular beverages worldwide, whose production and consumption result in large amounts of waste, namely spent coffee grounds, constituting an important source of compounds for several industrial applications. This work focused on the establishment of the volatile fingerprint of five spent coffee grounds from different geographical origins using headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME/GC-MS), as a strategy to identify volatile organic metabolites (VOMs) with potential application in the food industry as antioxidant, anti-inflammatory, and antiproliferative agents. One hundred eleven VOMs belonging to different chemical families were identified, of which 60 were found in all spent coffee grounds analyzed. Furanic compounds (34%), nitrogen compounds (30%), and esters (19%) contributed significant to the total volatile fingerprint. The data obtained suggest that spent coffee grounds have great potential to be used as raw material for different approaches in the food industry towards the development of new food ingredients or products for human consumption, in addition to pharmaceutical and cosmetic applications, namely as antioxidant (e.g., limonene, carvacrol), antimicrobial (e.g., pyrrole-2-carboxaldehyde, β-myrcene) and anti-inflammatory (e.g., furfural, 2-furanmethanol) agents, promoting their integral valorization within the circular bioeconomy concept.

Green extraction techniques (GreETs) emerged in the last decade as greener and sustainable alternatives to classical sample preparation procedures aiming to improve the selectivity and sensitivity of analytical methods, simultaneously reducing the deleterious side effects of classical extraction techniques (CETs) for both the operator and the environment. The implementation of improved processes that overcome the main constraints of classical methods in terms of efficiency and ability to minimize or eliminate the use and generation of harmful substances will promote more efficient use of energy and resources in close association with the principles supporting the concept of green chemistry. The current review aims to update the state of the art of some cutting-edge GreETs developed and implemented in recent years focusing on the improvement of the main analytical features, practical aspects, and relevant applications in the biological, food, and environmental fields. Approaches to improve and accelerate the extraction efficiency and to lower solvent consumption, including sorbent-based techniques, such as solid-phase microextraction (SPME) and fabric-phase sorbent extraction (FPSE), and solvent-based techniques (μQuEChERS; micro quick, easy, cheap, effective, rugged, and safe), ultrasound-assisted extraction (UAE), and microwave-assisted extraction (MAE), in addition to supercritical fluid extraction (SFE) and pressurized solvent extraction (PSE), are highlighted.

Food supply disruption and shortage verified during the current pandemic events are a scenario that many anticipate for the near future. The impact of climate changes on food production, the continuous decrease in arable land, and the exponential growth of the human population are important drivers for this problem. In this context, adding value to food waste is an obvious strategy to mitigate food shortages, but there is a long way to go in this field. Globally, it is estimated that one-third of all food produced is lost. This is certainly due to many different factors, but the lack of awareness of the consumer about the nutritional value of certain foods parts, namely peels and seeds, is certainly among them. In this review, we will unveil the nutritional and bioactive value of the waste discarded from the most important fresh fruit and vegetables consumed worldwide as a strategy to decrease food waste. This will span the characterization of the bioactive composition of selected waste from fruits and vegetables, particularly their seeds and peels, and their possible uses, whether in our diet or recycled to other ends.

Pesticides are chemicals used in agriculture to prevent insects, fungi, weeds, and other pests, from damaging crops. In addition, some types of pesticides are used after harvest as sprout suppressant agents help keeping the quality parameters of crops during storage. Nonetheless, its presence, even at trace levels, in food products is becoming a big challenge regarding human health. The current work aimed to develop and validate a sensitive and high-throughput analytical approach, based on a state-of-the-art microextraction technique—µQuEChERS, combined with ultra-high performance liquid chromatography equipped with a photodiode array detection system (UHPLC-PDA) to quantify isopropyl-N-(3-chlorophenyl) carbamate (chlorpropham), commonly used as efficient sprout suppressant stored potatoes, in raw and cooked potatoes cultivated in different geographical regions of Madeira Island (Portugal). Good results were obtained in terms of figures of the merit of the method, with correlation coefficients (R2) higher than 0.999 and recoveries between 94.5% to 125%. Method limit of detection (LOD) and limit of quantification (LOQ) were 0.14 μg/Kg and 0.43 μg/Kg, respectively, which are much lower than the accepted and legislated requirements by the European Union, which is 20 μg/Kg for chlorpropham. The concentration of chlorpropham in raw potatoes is significantly higher when compared to cooked samples, which revealed that the thermic treatment during cooking had a significant effect on its degradation. A significant decrease (90%, on average) was observed on chlorpropham levels.

Fish and other seafood products are essential dietary components that are highly appreciated and consumed worldwide. However, the high perishability of these products has driven the development of a wide range of processing, preservation, and analytical techniques. This development has been accelerated in recent years with the advent of the fourth industrial revolution (Industry 4.0) technologies, digitally transforming almost every industry, including the food and seafood industry. The purpose of this review paper is to provide an updated overview of recent thermal and nonthermal processing and preservation technologies, as well as advanced analytical techniques used in the seafood industry. A special focus will be given to the role of different Industry 4.0 technologies to achieve smart seafood manufacturing, with high automation and digitalization. The literature discussed in this work showed that emerging technologies (e.g., ohmic heating, pulsed electric field, high pressure processing, nanotechnology, advanced mass spectrometry and spectroscopic techniques, and hyperspectral imaging sensors) are key elements in industrial revolutions not only in the seafood industry but also in all food industry sectors. More research is still needed to explore how to harness the Industry 4.0 innovations in order to achieve a green transition toward more profitable and sustainable food production systems.

The urinary volatomic profiling of Indian cohorts composed of 28 lung cancer (LC) patients and 27 healthy subjects (control group, CTRL) was established using headspace solid phase microextraction technique combined with gas chromatography mass spectrometry methodology as a powerful approach to identify urinary volatile organic metabolites (uVOMs) to discriminate among LC patients from CTRL. Overall, 147 VOMs of several chemistries were identified in the intervention groups—including naphthalene derivatives, phenols, and organosulphurs—augmented in the LC group. In contrast, benzene and terpenic derivatives were found to be more prevalent in the CTRL group. The volatomic data obtained were processed using advanced statistical analysis, namely partial least square discriminative analysis (PLS-DA), support vector machine (SVM), random forest (RF), and multilayer perceptron (MLP) methods. This resulted in the identification of nine uVOMs with a higher potential to discriminate LC patients from CTRL subjects. These were furan, o-cymene, furfural, linalool oxide, viridiflorene, 2-bromo-phenol, tricyclazole, 4-methyl-phenol, and 1-(4-hydroxy-3,5-di-tert-butylphenyl)-2-methyl-3-morpholinopropan-1-one. The metabolic pathway analysis of the data obtained identified several altered biochemical pathways in LC mainly affecting glycolysis/gluconeogenesis, pyruvate metabolism, and fatty acid biosynthesis. Moreover, acetate and octanoic, decanoic, and dodecanoic fatty acids were identified as the key metabolites responsible for such deregulation. Furthermore, studies involving larger cohorts of LC patients would allow us to consolidate the data obtained and challenge the potential of the uVOMs as candidate biomarkers for LC.

The volatile profiles of eight saffron samples (seven cultivated and one spontaneous) grown in different geographical districts within the Campania region (southern Italy) were compared. Using headspace solid-phase microextraction coupled to gas chromatography–mass spectrometry (HS-SPME/GC-MS), overall, 80 volatiles were identified in the eight landraces. Among them, safranal and its isomers and other related compounds such as isophorones, which are not only key odorants but also pharmacologically active metabolites, have been detected in all the investigated samples. Principal Component Analysis performed on the volatiles’ compounds revealed that the spontaneous sample turned out to be an outlier. In particular, the volatile organic compounds (VOCs) profile of the spontaneous saffron presented four lilac aldehydes and four lilac alcohol isomers, which, to the authors’ knowledge, have never been identified in the volatile signature of this spice. The multivariate statistical analysis allowed the discrimination of the seven cultivate saffron ecotypes in four well-separated clusters according to variety. Moreover, 20 VOCs, able to differentiate the clusters in terms of single volatile metabolite, were discovered. Altogether, these results could contribute to identifying possible volatile signature metabolites (biomarkers) or patterns that discriminate saffron samples grown in Campania region on a molecular basis, encouraging future biodiversity programs to preserve saffron landraces revealing valuable genetic resources.

Worldwide, the food industry generates a large number of by-products from a wide variety of sources. These by-products represent an interesting and economical source of added value components with potential functionalities and/or bioactivities, which might be explored for industrial purposes, encouraging and promoting the circular economy concept. In this context, the current work aimed to evaluate the fatty acids (FAs) profile using gas chromatography–flame ionization detector (GC–FID) and Fourier Transform Infrared (FTIR), as well as the determination of related health lipid indices (e.g., atherogenic (AI) and thrombogenic (TI)) as a powerful strategy to investigate the potential applications of different agri-food by-products for human nutrition and animal feeding. This work results showed that polyunsaturated fatty acids (PUFAs) are the predominant group in grape pomace (72.7%), grape bunches (54.3%), and brewer’s spent grain (BSG, 59.0%), whereas carrot peels are dominated by monounsaturated fatty acids (MUFAs, 47.3%), and grape stems (46.2%), lees (from 50.8 to 74.1%), and potato peels (77.2%) by saturated fatty acids (SFAs). These findings represent a scientific basis for exploring the nutritional properties of agri-food by-products. Special attention should be given to grape pomace, grape bunches, and BSG since they have a high content of PUFAs (from 54.3 to 72.7%) and lower AI (from 0.11 to 0.38) and TI (from 0.30 to 0.56) indexes, suggesting their potential to provide a variety of health benefits against cardiovascular diseases including well-established hypotriglyceridemia and anti-inflammatory effects, products to which they are added.

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.

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.

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.

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.

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.

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.

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.

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 (

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.

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.

Tangerines (Citrus reticulata) are popular fruits worldwide, being rich in many bioactive metabolites. The setubalense variety cultivated on Madeira Island has an intense aroma easily distinguishable from other tangerines, being traditionally used to enrich several foods and beverages. Nonetheless, setubalense volatile composition has never been characterized, and we aimed to unveil the bioactive potential of peels and juices of setubalense tangerines and compare them with the murcott variety grown in Portugal mainland. Using headspace solid-phase microextraction coupled to gas chromatography mass spectrometry (HS-SPME/GC-MS), we identified a total of 128 volatile organic metabolites (VOMs) in the juice and peels, with d-limonene, γ-terpinene, β-myrcene, α- and β-pinene, o-cymene, and terpinolene, the most dominant in both cultivars. In contrast, setubalense juices are richer in terpenes, many of them associated with health protection. Discriminant analysis revealed a pool of VOMs, including β-caryophyllene and E-ocimene, with bioactive properties able to differentiate among tangerines according to variety and sample type (peel vs. juice). This is the first report on the volatile composition of setubalense tangerines grown on Madeira Island revealing that its pungent aroma is constituted by secondary metabolites with specific aroma notes and health properties. This is strong evidence of the higher nutraceutical value of such fruit for the human diet.