Search

This study addresses a comparative comprehensive metabolic profiling of two Egyptian cultivars of fenugreek (Trigonella foenum-graecum L.) seeds ‘Giza 2’ and ‘Giza 30’ via RP-HPLC-DAD-QTOF-MS and MS/MS. Briefly, 126 metabolites were detected in the samples under investigation, being classified into hydroxybenzoic acids (8), hydroxycinnamic acids (7), flavonoids (49 with a predominancy of flavones in particular apigenin derivatives), coumarins (1), furostanol saponins (17), alkaloids (2), amino acids (11), peptides (2), jasmonates (6), nucleosides (30), organic acids (16), terpenoids (1), and sugars (3). In addition, the total phenolic content and antioxidant activity were determined and compared with other geographically related seeds (chickpea Giza-1, sesame Giza-32, and linseed, Giza-10), showing slight differences among them but higher values than the other geographically related seeds that were segregated from them upon chemometric analysis. This is the first comprehensive metabolic profiling of these cultivars, presenting an initial account of some metabolites found in Fabaceae, such as apigenin di C pentoside, with a significant occurrence of biologically active furostanol saponins. It gives a prospect of fenugreeks richness of bioactive metabolites as an essential functional food that could add value to the food and nutraceutical industries' sustainability.

Cocoa pod husk (CPH) and cocoa bean shell (CBS) are by-products obtained during pre-processing and processing of cocoa beans. Several bioactive compounds have been identified in these by-products that can be used for commercial applications as a way to promote the circular economy. Therefore, the objective of this paper was to recover bioactive compounds from CPH and CBS by sonoextraction process, to determine the type, content, and antioxidant activity in optimized extracts. To achieve our purpose, an optimization strategy using Box-Behnken Design coupled response surface methodology (MRS) was applied. The extraction conditions were optimized. The results obtained for CBS were: TPC (193 mg GAE/g), TEAC (1.02 mmol TE/g), FRAP (1.02 mmol FeSO4/g) and ORAC (2.6 mmol TE/g), while for CPH, the reported values were: TPC (48 mg GAE/g), TEAC (0.30 mmol TE/g), FRAP (0.35 mmol FeSO4/g) and ORAC (0.43 mmol TE/g) under the optimized conditions: Time (XA): 15 min, Amplitude (XB): 80 %, Ethanol (XC): 50 %. The LC-ESI-qTOF-MS analysis results allowed the identification of 79 compounds, of which 39 represent the CBS extract, while 40 compounds were identified in CPH extract. To conclude, sonotrode based extraction could be considered as an efficient and fast alternative for the recovery of bioactive substances from CBS and CPH.

Abstract The objective of this study was to optimize different vacuum drying conditions for cocoa pod husk and cocoa bean shell in order to enhance these by-products for commercial applications. To carry out the optimization, the response surface methodology was applied using a Box–Behnken experimental design with 15 experiments for which different conditions of temperature (X1), drying time (X2) and vacuum pressure (X3) were established. The response variables were the content of total polyphenols, the content of flavanols and the radical scavenging activity evaluated in the extracts of the different experiments. Temperature (50–70 °C), drying time (3–12 h) and vacuum pressure (50–150 mbar) were considered as independent variables. The main factors affecting the response variables were temperature, followed by vacuum pressure. For the content of polyphenols, the optimal response values predicted for the cocoa pod husk was 11.17 mg GAE/g with a confidence limit (95%) of 9.05 to 13.28 mg GAE/g (optimal conditions: 65 °C, 8 h and 75 mbar), while for the cocoa bean shell cocoa was 29.61 mg GAE/g with a confidence limit (95%) of 26.95 to 32.26 mg GAE/g (optimal conditions: 50 °C, 5 h and 100 mbar). Therefore, results of this study suggest a high content of phenolic compounds obtained from these by-products that show relevance as functional ingredients for application in the food, nutraceutical, and cosmeceutical industries.

Cherry stems, prized in traditional medicine for their potent antioxidant and anti-inflammatory properties, derive their efficacy from abundant polyphenols and anthocyanins. This makes them an ideal option for addressing skin aging and diseases. This study aimed to assess the antioxidant and anti-inflammatory effects of cherry stem extract for potential skincare use. To this end, the extract was first comprehensively characterized by HPLC-ESI-qTOF-MS. The extract’s total phenolic content (TPC), antioxidant capacity, radical scavenging efficiency, and its ability to inhibit enzymes related to skin aging were determined. A total of 146 compounds were annotated in the cherry stem extract. The extract effectively fought against NO· and HOCl radicals with IC50 values of 2.32 and 5.4 mg/L. Additionally, it inhibited HYALase, collagenase, and XOD enzymes with IC50 values of 7.39, 111.92, and 10 mg/L, respectively. Based on the promising results that were obtained, the extract was subsequently gently integrated into a cosmetic gel at different concentrations and subjected to further stability evaluations. The accelerated stability was assessed through temperature ramping, heating-cooling cycles, and centrifugation, while the long-term stability was evaluated by storing the formulations under light and dark conditions for three months. The gel formulation enriched with cherry stem extract exhibited good stability and compatibility for topical application. Cherry stem extract may be a valuable ingredient for creating beneficial skincare cosmeceuticals.

Plant extracts rich in phenolic compounds have been reported to exert different bioactive properties. Despite the fact that there are plant extracts with completely different phenolic compositions, many of them have been reported to have similar beneficial properties. Thus, the structure–bioactivity relationship mechanisms are not yet known in detail for specific classes of phenolic compounds. In this context, this work aims to demonstrate the relationship of extracts with different phenolic compositions versus different bioactive targets. For this purpose, five plant matrices (Theobroma cacao, Hibiscus sabdariffa, Silybum marianum, Lippia citriodora, and Olea europaea) were selected to cover different phenolic compositions, which were confirmed by the phytochemical characterization analysis performed by HPLC-ESI-qTOF-MS. The bioactive targets evaluated were the antioxidant potential, the free radical scavenging potential, and the inhibitory capacity of different enzymes involved in inflammatory processes, skin aging, and neuroprotection. The results showed that despite the different phenolic compositions of the five matrices, they all showed a bioactive positive effect in most of the evaluated assays. In particular, matrices with very different phenolic contents, such as T. cacao and S. marianum, exerted a similar inhibitory power in enzymes involved in inflammatory processes and skin aging. It should also be noted that H. sabdariffa and T. cacao extracts had a low phenolic content but nevertheless stood out for their bioactive antioxidant and anti-radical capacity. Hence, this research highlights the shared bioactive properties among phenolic compounds found in diverse matrices. The abundance of different phenolic compound families highlights their elevated bioactivity against diverse biological targets.

The taste of food plays a crucial role in determining what and how much we eat. Thus, interventions that temporarily block sweet taste receptors offer a promising approach to addressing unhealthy behaviours associated with sugary foods. However, the relationship between reduced sweet taste response and food consumption remains unclear, with contradictory findings. Certain studies suggest that a diminished perception of sweetness leads to a sense of fullness and results in reduced food intake, while others suggest the opposite effect. To shed some light, our systematic review looked into the relationship between diminished sweet taste response and food consumption by examining the effects of bioactive compounds that experimentally inhibit sweetness in healthy individuals. This review was registered in the International Prospective Register of Systematic Reviews and conducted according to the Preferred Reporting Items for Systematic Reviews and Meta-Analyses (PRISMA) and the Scottish Intercollegiate Guidelines Network, and covered original papers included in Web of Science, PubMed, Scopus, Food Science Source and Food Science and technology abstracts. We identified 33 peer-reviewed English-language studies that fit the topic and met the inclusion criteria. The current literature predominantly focuses on the immediate impact of oral gymnemic acids, failing to provide preliminary evidence in support of the specific threshold hypothesis, above which food consumption decreases and below which the opposite effect occurs. Additionally, there was inconsistency in the findings regarding the short-term desire to eat following sweetness inhibition. Considering the downstream effects on energy intake and their clinical applications, further research is needed to clarify both the acute within-session effects (i.e., not wanting any more now) and the longer-term effects (i.e., deciding not to start eating) linked to oral sweet-taste-suppressing compounds.

This article, the second in a two-part series, continues the discussion on the nature of the relationship between the level of sweet taste suppression and eating behaviour, but in animal rather human subjects. In particular, the aim was to review the scientific literature on the impact that bioactive compounds that decrease oral sweet sensations have on intake, preference and physiological status in preclinical studies. This review was registered in the International Prospective Register of Systematic Reviews and conducted according to the Preferred Reporting Items for Systematic Reviews and Meta-Analyses (PRISMA) and the Scottish Intercollegiate Guidelines Network and covered original papers included in Web of Science, PubMed, Scopus, Food Science Source and Food Science and technology abstracts. We identified 28 peer-reviewed English-language studies that fit the topic and met the inclusion criteria. We identified three plant species, Gymnema sylvestre, Hovenia dulcis, and Ziziphus jujuba, that possess acute sweetness-inhibitory properties. When administered orally, these plants reduced neural responses to sweet stimuli and decreased consumption. However, studies on the longer-term effects of antisweet activity remain to be conducted. Translating the valuable insights into the mechanisms underlying the relationship between sweet taste impairment and eating behaviour into practical clinical applications are discussed.

Excessive consumption of added sugars is linked to chronic diseases, such as obesity, diabetes, dyslipidaemia or cardiovascular disease; and public health is searching for new strategies to reduce it. Although plant-derived bioactive compounds with inhibitory properties of sweet taste like Gymnema sylvestre show the potential to reduce sugar intake acutely, their impact after repeated administration is unknown. Therefore, we examined the changes of single and repeated exposures of a Gymnema sylvestre constituent, gurmarin, in sweet beverage consumption and preference in a preclinical model. 24 Wistar rats (50 % females) were divided into experimental (gurmarin) and two control groups (gymnemic acids or phosphate buffer solutions) according to the substances orally applied. Then acceptance and preference tests with sugar were performed within (Experiment 1) and between sessions (Experiment 2). We found that administering gurmarin decreased sucrose intake significantly, even after multiple treatments, without rebound effects. These findings suggest that sweet taste suppressors could be an effective tool for reducing long-term sugar consumption when repeatedly administrated.

Background Prior evidence suggests that capsinoids ingestion may increase resting energy expenditure (EE) and fat oxidation (FATox), yet whether they can modulate those parameters during exercise conditions remains poorly understood. We hypothesized that dihydrocapsiate (DHC) ingestion would increase EE and specifically FATox during an acute bout of aerobic exercise at FATmax intensity (the intensity that elicits maximal fat oxidation during exercise [MFO]) in men with overweight/obesity. Since FATmax and MFO during aerobic exercise appear to be indicators of metabolic flexibility, whether DHC has an impact on FATox in this type of population is of clinical interest. Methods A total of 24 sedentary men (age = 40.2 ± 9.2 years-old; body mass index = 31.6 ± 4.5 kg/m2 [n = 11 overweight, n = 13 obese]) participated in this randomized, triple-blinded, placebo-controlled, crossover trial (registered under ClinicalTrials.gov Identifier no. NCT05156697). On the first day, participants underwent a submaximal exercise test on a cycle ergometer to determine their MFO and FATmax intensity during exercise. After 72 hours had elapsed, the participants returned on 2 further days (≥ 72 hours apart) and performed a 60 min steady-state exercise bout (i.e. cycling at their FATmax, constant intensity) after ingesting either 12 mg of DHC or placebo; these conditions were randomized. Respiratory gas exchange was monitored by indirect calorimetry. Serum marker concentrations (i.e. glucose, triglycerides, non-esterified fatty acids (NEFAs), skin temperature, thermal perception, heart rate, and perceived fatigue) were assessed. Results There were no significant differences (P > 0.05) between DHC and placebo conditions in the EE and FATox during exercise. Similarly, no significant changes were observed in glucose, triglycerides, or NEFAs serum levels, neither in the skin temperature nor thermal perception across conditions. Heart rate and perceived fatigue did not differ between conditions. Conclusions DHC supplementation does not affect energy metabolism during exercise in men with overweight/obesity.

Inflammatory bowel disease (IBD) is a chronic gastrointestinal inflammation with unpredictable symptom fluctuations. While there is no effective cure for IBD, various treatments aim to manage symptoms and improve the quality of life for affected individuals. In recent years, there has been growing interest in the potential benefits of certain natural plants and herbs in the management of IBD. In this regard, this study aimed to evaluate the immunomodulatory and anti-inflammatory effects of a well-characterized extract of Salvia verbenaca (S. verbenaca) in an experimental model of colitis in rats. Interestingly, the daily administration of S. verbenaca (10 and 25 mg/kg) effectively alleviated colitis symptoms, as evidenced by reduced weight/length ratio and colonic damage. Moreover, it reduced oxidative stress markers (MPO and GSH), decreased pro-inflammatory cytokine expression (Il-6, Il-12a, Il-1β, Il-23, Icam-1, Mcp-1, Cinc-1), and preserved the integrity of the intestinal barrier (Villin, Muc-2, Muc-3). These effects suggest S. verbenaca extract could represent a potential complementary candidate to treat gastrointestinal disorders. Its beneficial actions can be related to its antioxidant properties as well as the downregulation of the immune response, which can result in the improvement in the intestine epithelial barrier.

Bioactive compounds are found in foods in small quantities and represent extra nutritional constituents known to exert beneficial effects on health beyond their nutritional value [...]

The constant growth of the cosmetic industry, together with the scientific evidence of the beneficial properties of phytochemicals, has generated great interest in the incorporation of bioactive extracts in cosmetic formulations. This study aims to evaluate the bioactive potential of a mango peel extract for its incorporation into cosmetic formulations. For this purpose, several assays were conducted: phytochemical characterization; total phenolic content (TPC) and antioxidant potential; free-radical scavenging capacity; and skin aging-related enzyme inhibition. In addition, the extract was incorporated into a gel formulation, and a preliminary stability study was conducted where the accelerated (temperature ramp, centrifugation, and heating/cooling cycles) and long-term (storage in light and dark for three months) stability of the mango peel formulations were evaluated. The characterization results showed the annotation of 71 compounds, gallotannins being the most representative group. In addition, the mango peel extract was shown to be effective against the •NO radical with an IC50 of 7.5 mg/L and against the hyaluronidase and xanthine oxidase enzymes with IC50 of 27 mg/L and 2 mg/L, respectively. The formulations incorporating the extract were stable during the stability study. The results demonstrate that mango peel extract can be a by-product to be revalorized as a promising cosmetic ingredient.

Abstract A gain-of-function mutation in the fibroblast growth factor receptor 3 gene (FGFR3) results in achondroplasia (ACH), the most frequent form of dwarfism. Constitutive activation of FGFR3 impairs bone formation and elongation and many signal transduction pathways. Identification of new and relevant compounds targeting the FGFR3 signaling pathway is of broad importance for the treatment of ACH, and natural plant compounds are prime drug candidate sources. Here, we found that the phenolic compound (-)-epicatechin, isolated from Theobroma cacao, effectively inhibited FGFR3’s downstream signaling pathways. Transcriptomic analysis in an Fgfr3 mouse model showed that ciliary mRNA expression was modified and influenced significantly by the Indian hedgehog and PKA pathways. (-)-Epicatechin is able to rescue mRNA expression impairments that control both the structural organization of the primary cilium and ciliogenesis-related genes. In femurs isolated from a mouse model (Fgfr3 Y367C/+ ) of ACH, we showed that (-)-epicatechin eliminated bone growth impairment during 6 days of ex vivo culture. In vivo, we confirmed that daily subcutaneous injections of (-)-epicatechin to Fgfr3 Y367C/+ mice increased bone elongation and rescued the primary cilium defects observed in chondrocytes. This modification to the primary cilia promoted the typical columnar arrangement of flat proliferative chondrocytes and thus enhanced bone elongation. The results of the present proof-of-principle study support (-)-epicatechin as a potential drug for the treatment of ACH.

Abstract Background Succinate is produced by both host and microbiota, with a key role in the interplay of immunity and metabolism and an emerging role as a biomarker for inflammatory and metabolic disorders in middle-aged adults. The relationship between plasma succinate levels and cardiovascular disease (CVD) risk in young adults is unknown. Methods Cross-sectional study in 100 (65% women) individuals aged 18–25 years from the ACTIvating Brown Adipose Tissue through Exercise (ACTIBATE) study cohort. CVD risk factors, body composition, dietary intake, basal metabolic rate, and cardiorespiratory fitness were assessed by routine methods. Plasma succinate was measured with an enzyme-based assay. Brown adipose tissue (BAT) was evaluated by positron emission tomography, and circulating oxylipins were assessed by targeted metabolomics. Fecal microbiota composition was analyzed in a sub-sample. Results Individuals with higher succinate levels had higher levels of visceral adipose tissue (VAT) mass (+ 42.5%), triglycerides (+ 63.9%), C-reactive protein (+ 124.2%), diastolic blood pressure (+ 5.5%), and pro-inflammatory omega-6 oxylipins than individuals with lower succinate levels. Succinate levels were also higher in metabolically unhealthy individuals than in healthy overweight/obese peers. Succinate levels were not associated with BAT volume or activity or with fecal microbiota composition and diversity. Conclusions Plasma succinate levels are linked to a specific pro-inflammatory omega-6 signature pattern and higher VAT levels, and seem to reflect the cardiovascular status of young adults.

Obesity is a worldwide public health problem whose prevalence rate has increased steadily over the last few years. Therefore, it is urgent to improve the management of obesity and its comorbidities, and plant-based treatments are receiving increasing attention worldwide. In this regard, the present study aimed to investigate a well-characterized extract of Lavandula multifida (LME) in an experimental model of obesity in mice and explore the underlying mechanisms. Interestingly, the daily administration of LME reduced weight gain as well as improved insulin sensitivity and glucose tolerance. Additionally, LME ameliorated the inflammatory state in both liver and adipose tissue by decreasing the expression of various proinflammatory mediators (Il-6, Tnf-α, Il-1β, Jnk-1, Pparα, Pparγ, and Ampk) and prevented increased gut permeability by regulating the expression of mucins (Muc-1, Muc-2, and Muc-3) and proteins implicated in epithelial barrier integrity maintenance (Ocln, Tjp1, and Tff-3). In addition, LME showed the ability to reduce oxidative stress by inhibiting nitrite production on macrophages and lipid peroxidation. These results suggest that LME may represent a promising complementary approach for the management of obesity and its comorbidities.

The goal of this work was to monitor the hydrophilic profile of the virgin olive oil (VOO) of the second main Tunisian variety, “Chétoui”, in order to achieve a better understanding of the behavior of the bioactive phenolic compounds during 0, 2, 5, 10, and 15 min of microwave heating at medium power 800 W, and 0, 2.5, and 5 h of conventional heating at 180 °C. The extent of the oxidative and hydrolytic degradation of the different phenolic subclasses was evaluated using high-performance liquid chromatography (HPLC) coupled to electrospray time-of-flight mass spectrometry (TOF-MS) method. During heating process, the most represented component in Chétoui VOO was found to be isomer 1 and 2 of deacetoxy oleuropein aglycone, and hydroxy decarboxy oleuropein aglycon. These compounds may be considered as direct markers for the degree of transformation of secoiridoids during heating process. Among the studied phenolic compounds, hydroxytyrosol, tyrosol, luteolin and apigenin displayed the highest heating resistance in the whole time range of microwave and conventional applications. However, the main secoiridoids quantified in the fresh VOO, isomer 2 of oleuropein aglycone, and ligstroside aglycone, decreased in concentration with the thermal treatment and this decrease was drastic under conventional heating. Keywords: Tunisian olive variety, Olive oil degradation, Thermo-oxidation, HPLC-ESI-TOF-MS, Phenolic compounds, Microwaves, Conventional oven

Paliurus spina-christi Mill., a member of the Rhamnaceae family, is a traditionally used medicinal plant in the management of a panoply of human ailments. The current research focused on its phytochemical profile and biological properties evaluated by its antioxidant and enzyme inhibitory properties. The methanol extract was found to be the most effective antioxidant as evidenced by its DPPH and ABTS scavenging activities, cupric and ferric reducing power (CUPRAC and FRAP), and high activity in phosphomolybdenum (PBD) assay, and also displayed the highest anti-tyrosinase activity. The n-hexane extract was the most effective AChE inhibitor (8.89 ± 0.08 mg GALAE/g) followed by the methanol (8.64 ± 0.01 mg GALAE/g) while the latter showed the highest BChE inhibition (2.50 ± 0.05 mg GALAE/g). Among the different solvent extracts of the stem, the methanolic extract showed highest antioxidant activity in the following assays: DPPH (909.88 ± 4.25 mg TE/g), ABTS (3358.33 ± 51.14 mg TE/g), CUPRAC (781.88 ± 16.37 mg TE/g), FRAP (996.70 ± 47.28 mg TE/g), and PBD (4.96 ± 0.26 mmol TE/g), while the dichloromethane extract showed the highest MCA (28.80 ± 0.32 mg EDTAE/g). The methanol extracts revealed the highest TPC and TFC among the different solvents used, and as for plant part, the stem extracts had the highest TPC ranging from 22.36 ± 0.26 to 121.78 ± 1.41 (mg GAE/g), while the leaf extracts showed the highest TFC ranging from 8.43 ± 0.03 to 75.36 ± 0.92 (mg RE/g). Our findings tend to provide additional scientific evidence on the biological and chemical activities of P. spina-christi, which may serve as a source of naturally occurring bioactive chemicals with potential biomedical applications.

Neurodegenerative diseases are known for their wide range of harmful conditions related to progressive cell damage, nervous system connections and neuronal death. These pathologies promote the loss of essential motor and cognitive functions, such as mobility, learning and sensation. Neurodegeneration affects millions of people worldwide, and no integral cure has been created yet. Here, bioactive compounds have been proven to exert numerous beneficial effects due to their remarkable bioactivity, so they could be considered as great options for the development of new neuroprotective strategies. Phenolic bioactives have been reported to be found in edible part of plants; however, over the last years, a large amount of research has focused on the phenolic richness that plant by-products possess, which sometimes even exceeds the content in the pulp. Thus, their possible application as an emergent neuroprotective technique could also be considered as an optimal strategy to revalorize these agricultural residues (those originated from plant processing). This review aims to summarize main triggers of neurodegeneration, revise the state of the art in plant extracts and their role in avoiding neurodegeneration and discuss how their main phenolic compounds could exert their neuroprotective effects. For this purpose, a diverse search of studies has been conducted, gathering a large number of papers where by-products were used as strong sources of phenolic compounds for their neuroprotective properties. Finally, although a lack of investigation is quite remarkable and greatly limits the use of these compounds, phenolics remain attractive for research into new multifactorial anti-neurodegenerative nutraceuticals.

Strokes are the second most common cause of death worldwide and a leading cause of disability. Regular consumption of polyphenols has been shown to reduce the risk of suffering a cardiovascular event. For this reason, we have investigated the protective effect of Salicornia ramosissima, a seasonal halophyte that synthetizes high amounts of bioactive compounds, including polyphenols, in response to environmental stress. Aqueous, hydroalcoholic, and ethanolic extracts were prepared to investigate if dietary supplementation prior to ischemic challenge can prevent subsequent damage using two animal models. First, we screened the protective effect against hypoxia–reoxygenation in Drosophila melanogaster and observed that both ethanolic and hydroalcoholic extracts protected flies from the deleterious effects of hypoxia. Second, we confirmed the protective effect of S. ramosissima ethanolic extract against brain ischemia using the transient middle cerebral artery occlusion mice model. Four weeks of oral supplementation with the ethanolic extract before artery occlusion reduced infarct volume and lowered the plasma levels of the DNA peroxidant product 8-hydroxydeoxyguanosine. Phytochemical profiling of S. ramosissima ethanolic extract revealed 50 compounds. Thus, it represents a valuable source of bioactive compounds that show promising disease-modifying activities and could be further developed as an effective food supplement for the prevention or treatment of neurovascular disorders.

Recent years have seen a rise in the popularity of the consumption of sports-related supplements. However, the hypothesis is raised that it is necessary to analyze the quality aspects of these supplements in relation to the information provided on the label, to avoid associated risks and obtain the greatest possible benefit from their consumption. Therefore, the aim of this study has been to carry out an analysis or screening of the protein supplements that are currently marketed in Spain. We analyzed the labels of 52 protein sports supplements available both in physical stores and online. The analysis consisted of addressing three relevant aspects considering the labeling: (a) the legislative framework in which the supplements are marketed, (b) the quality of the protein, and (c) the presence of other ingredients according to the specifications of the label. In the legislative context, there do not seem to be any specific regulations to guarantee consumer protection, which can lead to unfair practices and misleading advertising. Most of the supplements analyzed to comply with the requirements of their current regulations. However, claims about their benefits that are not allowed under European legislation have been found in some of them. Regarding composition and according to label information, the supplements have been found to provide a sufficient dose of protein in terms of recommended protein intake per serving. Regarding the presence of other ingredients and according to the information on the label, most of them, except for egg supplements, contain other ingredients. Colostrum was also found in one of the supplements evaluated. The conclusions of the study reveal that, due to a lack of knowledge or misleading advertising practices, supplements are often not used properly. The information provided is essential for both professionals and consumers to avoid the risks associated with consumption, such as unintentional doping, interactions between ingredients that reduce the quality of the supplement, and consumption of supplements inappropriately, among others.

The present study is aimed at valorizing grape pomace, one of the most abundant winery-making by-products of the Mediterranean area, through the extraction of the main bioactive compounds from the skin of grape pomace and using them to manufacture innovative nanoformulations capable of both avoiding skin damages and promoting skincare. The phytochemicals were recovered through maceration in hydroethanolic solution. Catechin, quercetin, fisetin and gallic acid, which are known for their antioxidant power, were detected as the main compounds of the extract. Liposomes and phospholipid vesicles modified with glycerol or Montanov 82® or a combination of both, were used as carriers for the extract. The vesicles were small (~183 nm), slightly polydispersed (PI ≥ 0.28), and highly negatively charged (~−50 mV). The extract was loaded in high amounts in all vesicles (~100%) irrespective of their composition. The antioxidant activity of the extract, measured by using the DPPH (2,2-Diphenyl-1-picrylhydrazyl) test, was 84 ± 1%, and slightly increased when loaded into the vesicles (~89%, P

Asparagus officinalis L. is a common vegetable widely consumed due to its high consumer acceptance. In addition to its flavor, green asparagus contains a high amount of bioactive compounds with health-promoting effects. In this sense, the growing concern of the public health system to promote a diet with a higher consumption of vegetables makes research on phytochemicals from this food of interest. In order to study the content of bioactive compounds from plant matrices, the combination of advanced extraction and analytical techniques within the context of green chemistry is an indispensable working model in today’s research. In the present experimental work, the composition of the phytochemicals of green asparagus from the Protected Geographical Indication (PGI) located in Huétor Tájar, Granada (Spain), was evaluated by environmentally friendly extraction techniques. In order to carry out this work, the recovery of bioactive compounds was evaluated by pressurized liquid extraction (PLE) using GRAS (Generally Recognized As Safe) solvents (mixtures of water and ethanol). The extraction was optimized using a Response Surface Methodology (RSM) based on a 24 factorial Central Composite Design (CCD). The experimental model was followed by high-performance liquid chromatography coupled to electrospray ionization time-of-flight mass spectrometry (HPLC–ESI-TOF-MS) analytical methodology for a comprehensive characterization. The optimized methodology was compared with conventional solid–liquid extraction protocols using ethanol and water. The results highlighted the potential of advanced PLE techniques compared to conventional systems for the recovery of green asparagus phytochemicals. Moreover, the analytical characterization allowed the identification and quantitation of major phenolic compounds belonging to phenolic acids and flavonoids families. Therefore, an easy, fast, and novel methodology to optimize the extraction of bioactive compounds from green asparagus has been optimized, using Green and GRAS methodology, which enables a better understanding of the bioactive composition of this widely consumed food.

The aim of the present study is to investigate the phytochemical composition of tiger nut (TN) (Cyperus esculentus L.) and its neuroprotective potential in scopolamine (Scop)-induced cognitive impairment in rats. The UHPLC-ESI-QTOF-MS analysis enabled the putative annotation of 88 metabolites, such as saccharides, amino acids, organic acids, fatty acids, phenolic compounds and flavonoids. Treatment with TN extract restored Scop-induced learning and memory impairments. In parallel, TN extract succeeded in lowering amyloid beta, β-secretase protein expression and acetylcholine esterase (AChE) activity in the hippocampus of rats. TN extract decreased malondialdehyde levels, restored antioxidant levels and reduced proinflammatory cytokines as well as the Bax/Bcl2 ratio. Histopathological analysis demonstrated marked neuroprotection in TN-treated groups. In conclusion, the present study reveals that TN extract attenuates Scop-induced memory impairments by diminishing amyloid beta aggregates, as well as its anti-inflammatory, antioxidant, anti-apoptotic and anti-AChE activities.

The avocado is one of the most produced and consumed tropical fruits worldwide, so more than 1.5 million tons of waste are generated per year, especially due to its main by-products: the seed and peel. In order to demonstrate whether these extracts are able to exert health benefits related to oxidative stress, a series of in vitro tests were conducted: an identification and quantification using HPLC, and an evaluation of the antioxidant capacity and ability to inhibit enzymatic overactivation. In the end, the avocado peel stood out as the more antioxidant extract, due to its higher phenolic content. However, both extracts can be considered as great options for developing new, high added-value products.

Custard apple (Annona cherimola Mill.) is a tropical fruit source of bioactive compounds whose main producer worldwide is Andalusia, Spain. Because of its processing, the food industry generates large amounts of by-products, such as peels and seeds. These by-products are rich in phenolic compounds with high antioxidant, anti-inflammatory and anti-aging powers. The objective of this work is to evaluate, by different in vitro methods, the antioxidant and anti-inflammatory potential of cherimoya by-products rich in phenolic compounds for the development of cosmeceuticals. In addition, the major phenolic compounds present in the custard apple peel and seed samples were characterized by HPLC-ESI-QTOF-MS. The results showed that both the peel and seed of custard apple have a strong potential against oxidative stress and inflammation. Its phytochemical profile due to the presence of phenolic compounds (catechin, epicatechin, rutin, quinic acid, vanillic acid, etc.) makes both industrial by-products attractive bioactive ingredients for the manufacture of functional food and cosmeceuticals.

In recent years, green and advanced extraction technologies have gained great interest to revalue several food by-products. This by-product revaluation is currently allowing the development of high value-added products, such as functional foods, nutraceuticals, or cosmeceuticals. Among the high valued-added products, cosmeceuticals are innovative cosmetic formulations which have incorporated bioactive natural ingredients providing multiple benefits on skin health. In this context, the extraction techniques are an important step during the elaboration of cosmetic ingredients since they represent the beginning of the formulation process and have a great influence on the quality of the final product. Indeed, these technologies are claimed as efficient methods to retrieve bioactive compounds from natural sources in terms of resource utilization, environmental impact, and costs. This review offers a summary of the most-used green and advanced methodologies to obtain cosmetic ingredients with the maximum performance of these extraction techniques. Response surface methodologies may be applied to enhance the optimization processes, providing a simple way to understand the extraction process as well as to reach the optimum conditions to increase the extraction efficiency. The combination of both assumes an economic improvement to attain high value products that may be applied to develop functional ingredients for cosmetics purposes.

Annona cherimola fruit, known as cherimoya or custard apple, is an exotic fruit from South America but is strongly produced in Andalusia, Spain. Its by-products (seeds and peel) are recognised as important sources of antioxidants, including phenolic acids, flavonoids and procyanidins. Therefore, the aim of this study was to carry out the characterization of its phenolic composition and to in vitro evaluate the bioactivity of custard apple seed and peel. Therefore, high performance liquid chromatography coupled to mass spectrometry (HPLC-ESI-qTOF-MS) was performed in order to tentatively identify their phenolic composition. In the end, 19 compounds were identified and quantified, some of them for the first time in the custard apple matrix. Then, seed and peel total phenolic content, as well as antioxidant properties, radical scavenging capacity (O2, NO, HOCl) and inhibition of enzymes involved in different pathologies (hyaluronidase, elastase, collagenase, tyrosinase, acetylcholinesterase and xanthine oxidase), were evaluated. Although both extracts showed almost similar antioxidant capacities, custard apple seed stood out slightly more than peel (171 ± 2 vs. 130.0 ± 0.4 μmol TE/g DE, resp.), especially as ·NO scavenger (IC50 1.5 ± 0.2 vs. 11.8 ± 0.3 mg/L, resp.) and hyaluronidase inhibitor (IC50 170 ± 10 vs. 460 ± 20mg/L, resp.). Finally, the application of extracts on a real human model of platelet aggregation was performed, reporting antiaggregatory effects in agonist-promoted platelet thrombus formation. All these results show that custard apple by-products are stated as interesting sources of bioactive compounds with multiple industrial applications for the development of high-added-value products, such as functional foods, nutraceuticals and cosmeceuticals, promoting the circular bioeconomy of these by-products.

Grapevine-derived products have been widely studied for their reported benefits, especially those related to the prevention of cardiovascular diseases. However, in recent years, the interest in the study of grapes and their non-fermented derivatives (grape juices) has gained prominence over the well-known interest in red wine, since grapes and grape juices seem to be widely related to the beneficial effects associated with the Mediterranean diet, and consequently to the presence of phenolic compounds. The focus of this systematic review was the phenolic profiles of grape, juice, and wine, as well as the possible beneficial effects of their consumption on the human microbiota through a systematic literature review. PubMed and Scopus were accessed during April 2021 and the PRISMA methodological protocol was followed. To the best of our knowledge, this is the first time that the PRISMA methodology has been applied to this systematic knowledge. This methodology allowed for a scientific description of: (a) the comparison between grapes and their derived products as source of phenolic compounds, (b) great possibilities for working on a new line of investigation based on the synergy between polyphenol consumption and microbiota, and (c) the urgent need for strategies to improve the bioavailability of these compounds.

Tradescantia is a genus of herbaceous and perennial plants belonging to the Commelinaceae family and organized into three infrageneric classifications and 12 sections. More than 80 species within the genus have been used for centuries for medicinal purposes. Phytochemical compounds (from various species of the genus) such as coumarins, alkaloids, saponins, flavonoids, phenolics, tannins, steroids and terpenoids have recently been characterized and described with antioxidant, cytotoxic, anti-inflammatory, anticancer or antimicrobial properties. The objective of this review is to describe the different aspects of the genus Tradescantia, including its botanical characteristics, traditional uses, phytochemical composition, biological activities, and safety aspects.

Medicinal and aromatic plants (MAPs) are potential sources of natural bioactive phytochemical compounds of an incredible worth for the food industry, such as polyphenols. Lamiaceae medicinal and aromatic plants from Granada’s high plateau, concretely Origanum bastetanum, Thymus zygis gracilis, Thymus longiflorus, Thymus membranaceus and Ziziphora hispanica, were evaluated under different conventional solid–liquid extraction conditions to obtain extracts enriched in bioactive compounds. Phenolic profile was detected by HPLC-QTOF-MS, identifying a high abundance of bioactive constituents. Furthermore, antioxidant and antiviral activities of the mentioned plants were studied as biological properties of interest for the improvement of food shelf-life. Thus, Origanum bastetanum showed the highest antioxidant potential for all assays. Antiviral activity was also tested against some important foodborne viruses, feline calicivirus (FCV), murine norovirus (MNV) and hepatitis A virus (HAV), with the highest activity obtained for Ziziphora hispanica, Thymus longiflorus and Origanum bastetanum. This research proposes the studied plants as rich sources of bioactive compounds with potential use as preservatives in the food industry.

Avocado seed and peel are the main by-products from avocado industrialisation, and account for nearly 30% of fruit weight. Although they are usually discarded, their high phenolic content has been deeply associated with several nutritional and functional benefits. Thus, for a comprehensive analytical evaluation of both semi-industrial extracts, various steps have been developed: tentative characterisation and quantification of the phenolic composition using HPLC-ESI-qTOF-MS, determination of TPC and antioxidant activity by Folin–Ciocalteu, FRAP, TEAC and ORAC methods, evaluation of scavenging capacity against different ROS and measurement of the enzymatic inhibitory potential against potentially harmful enzymes. Finally, their bioactive potential was tested in a human platelet model where antiaggregatory activity was measured. Hence, 48 different compounds were identified, where flavonoids and procyanidins were the most representative groups. The higher TPC was found in avocado peel extract (190 ± 3 mg/g), which showed more antioxidant power and more capacity to decrease ROS generation than seed extract (60 ± 2 mg/g). In addition, both extracts showed enzymatic inhibition, especially against hyaluronidase, xanthine oxidase and acetylcholinesterase. Lastly, avocado peel was proven to inhibit platelet aggregation with significant results at 1, 0.75 and 0.5 mg/mL, where the extract showed reducing effects on agonists’ expression such as p-selectin or GPIIb/IIIa complex. These results demonstrate that both semi-industrial extracts—above all, avocado peel—have an interesting potential to be exploited as a natural by-product with antioxidant properties with multiple applications for the prevention of different pathologies.

Nigella is a small genus of the family Ranunculaceae, which includes some popular species due to their culinary and medicinal properties, especially in Eastern Europe, Middle East, Western, and Central Asia. Therefore, this review covers the traditional uses and phytochemical composition of Nigella and, in particular, Nigella sativa. The pharmacological studies reported in vitro, in vivo, and in humans have also been reviewed. One of the main strength of the use of Nigella is that the seeds are rich in the omega-6 fatty acid linoleic acid and provide an extra-source of dietary phytochemicals, including the bioactive thymoquinone, and characteristics saponins, alkaloids, and flavonoids. Among Nigella species, N. sativa L. is the most studied plant from the genus. Due to the phytochemical composition and pharmacological properties, the seed and seed oil from this plant can be considered as good candidates to formulate functional ingredients on the basis of folklore and scientific knowledge. Nonetheless, the main limations are that more studies, especially, clinical trials are required to standardize the results, e.g. to establish active molecules, dosage, chemical profile, long-term effects and impact of cooking/incorporation into foods.

Olive leaves, one of the most abundant olive production by-products, have shown incredible potential for their characteristic bioactive compound composition, with unique compounds such as the polyphenol oleuropein. In order to evaluate the bioaccessibility of bioactive compounds present in an olive leaf extract, samples were submitted to an in vitro digestion process following INFOGEST protocol, and qualitative and quantitative characterization of the original extract and digestive samples at different times were carried out using HPLC-ESI-TOF-MS. The analyzed extract presented an abundance of phenolic compounds, such as secoiridoids, with oleuropein being the main identified compound. The in vitro digestion process showed an effect on the phenolic profile of the extract, with a lower recovery in the gastric phase and an increase at the beginning of the intestinal phase. Most of the studied compounds showed high bioaccessibility at the end of the digestion, with oleuropein, ligstroside, and quercetin-3-O-galactoside being among the ones with higher value. These findings show the potential for future use of olive leaf polyphenols. However, further research is needed in order to evaluate the absorption, delivery, and interaction of these compounds with the colon.

Mango consumption has shown bioactive properties against several diseases like diabetes, therefore, we evaluated how a mango-supplemented diet affects metabolic pathways in diabetic rats. Serum and liver samples were collected from 26 rats divided into 3 groups (healthy, untreated diabetic and mango-treated diabetic) after dietary intervention and analysed using an LC-MS untargeted metabolomic strategy. Twenty-six and 29 metabolites in serum and liver were potentially annotated, showing significant differences among groups. Several affected pathways were due to the disease state [fatty acids (i.e. palmitoleic, linolenic, stearidonic, eicosapentaenoic, docosahexaenoic acids and others), bile acids (i.e. glycocholic acid) and amino acids (i.e. leucine, isoleucine and valine)], and others due to mango supplementation (increased hepatic bioaccumulation of euxanthone, a mangiferin metabolite, and increased glutathione concentration). These results suggest that a mango-supplemented diet exerted a significant antioxidant effect in the liver of diabetic rats, likely due to its phenolic compounds, like mangiferin and its metabolites.

An investigation was conducted to study the beneficial effects of Ephedra alata monjauzeana crude extract (EamCE). The chemical profile was determined using RP-HPLC–ESI-QTOF-MS analysis, revealing the presence of twenty-one flavonoids and phenolic acids. A series of antioxidant assays was carried out using ten different methods. The EamCE has demonstrated a significant antioxidant potential, with interesting IC50 values not exceeding 40 µg/mL in almost activities. Likewise, a significant inhibition of key enzymes, involved in some health issues, such as Alzheimer’s disease, diabetes, hyperpigmentation, dermatological disorders, gastric/urinary bacterial infections, and obesity, was observed for the first time. The IC50 values ranged from 22.46 to 54.93. The anti-inflammatory and non-cytotoxic activities were assessed by heat-induced hemolysis and cell culture methods, respectively; the EamCE has shown a prominent effect in both tests, notably for the anti-inflammatory effect that was superior to the reference compound “diclofenac” (IC50: 71.03 ± 1.38 > 70.23 ± 0.99 (µg/mL)). According to these results, this plant could be used in a large spectrum as a food supplement, as a natural remedy for various physiological disorders and pathologies; and it might serve as a preventive and health care agent.

The study of the bioavailability of bioactive compounds is a fundamental step for the development of applications based on them, such as nutraceuticals, functional foods or cosmeceuticals. It is well-known that these compounds can undergo metabolic reactions before reaching therapeutic targets, which may also affect their bioactivity and possible applications. All recent studies that have focused on bioavailability and metabolism of phenolic and terpenoid compounds have been developed because of the advances in analytical chemistry and metabolomics approaches. The purpose of this review is to show the role of analytical chemistry and metabolomics in this field of knowledge. In this context, the different steps of the analytical chemistry workflow (design study, sample treatment, analytical techniques and data processing) applied in bioavailability and metabolism in vivo studies are detailed, as well as the most relevant results obtained from them.

The increasing production of tropical fruits followed by their processing results in tons of waste, such as skins or seeds. However, these by-products have been reported to be rich in bioactive compounds (BACs) with excellent properties of interest in the cosmeceutical industry: antioxidant, anti-aging, anti-inflammatory, antimicrobial and photoprotective properties. This review summarizes the tropical fruits most produced worldwide, their bioactive composition and the most important and studied therapeutic properties that their by-products can contribute to skin health, as well as the different approaches for obtaining these compounds using techniques by conventional (Soxhlet, liquid-liquid extraction or maceration) and non-conventional extractions (supercritical fluid extraction (SFE), ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE), pressurized liquid extraction (PLE) and two-phase aqueous system), followed by their identification by HPLC-MS or GC-MS analysis. Moreover, this work encompasses several studies that may prove the effects of seeds and skins from tropical fruits against oxidative stress, hyperpigmentation, acne, aging or UV radiation. Therefore, the investigation of functional components present in tropical fruit by-products under a circular bioeconomy model could be of great interest for the cosmeceutical industry and a very promising option for obtaining new cosmeceutical formulations.

Garlic (Allium sativum) has been described as containing phytonutrients with healthy properties. In this study, the effect of a bioactive garlic food supplement intake on human plasma metabolome was examined with the aim of understanding the mechanisms of action and involved pathways responsible for beneficial effects. With this purpose, a dietary intervention assay was performed in thirty healthy volunteers collecting plasma samples before intake and after one month of daily supplement consumption. Plasma samples were analysed by a fingerprinting metabolomic strategy based on HPLC-ESI-QTOF-MS. Our results revealed a total of 26 metabolites affected by supplement intake. In general, alterations in phospholipid metabolism were shown, detecting an increase in lysophosphatidylcholines, lysophosphatidylethanolamines and acylcarnitines. It is also remarkable that the level of four fructosamines decreased after the assay. These results are according with the antioxidant and antiglycation properties that have been previously associated with garlic extracts.

Recently, the relationship between nutrients and health is becoming since natural dietary products as polyphenols are being considered by their potential for the management of several diseases. We aimed to investigate the capacity of Lippia citriodora compounds to modulate AMP-activated protein kinase activity (AMPK) on a hypertrophic adipocyte model. HPLC semi-preparative purification method and reverse phase high performance liquid chromatography coupled to time-of-flight mass detection with electrospray ionization (RP-HPLC-ESI-TOF/MS) were used to obtain de compounds from L. citriodora extract. AMPK activity was measured on the hypertrophic 3T3-L1 adipocyte model by immunofluorescence microscopy. Four compounds of 29 total compounds have been tentatively identified in L. citriodora for the first time by HPLC-ESI-TOF-MS. Phenylpropanoids (verbascoside), iridoids (gardoside) and flavonoids (luteolin-7-diglucoronide) were the best candidates to account for activating AMPK capacity. The combination of specific polyphenols from L. citriodora, which showed strong activating AMPK capacity, could be an alternative in the management of obesity-associated diseases.

Phenolic compounds present in extra virgin olive oil (EVOO) could be retained in its byproducts during processing. Among them, hydroxytyrosol and its derivatives deserve special attention due to their health benefits recognized by The European Food Safety Authority (EFSA). In the present research, the presence of these compounds in the filter cake byproduct was studied by combining pressurized liquid extraction (PLE) and high-performance liquid chromatography coupled to time-of-flight mass spectrometry (HPLC-TOF-MS). The applied optimum extraction parameters were 1500 psi, 120 °C and aqueous ethanol (50:50, v/v). The influence of different drying methods (vacuum-, freeze- and spray-drying) in the recovery of phenolic compounds was also evaluated. A total of 16 compounds from EVOO were identified in the extracts, 3 of them being hydroxytyrosol-related compounds, 6 substances of oleoside and elenolic acid derivatives, together with 6 secoiridoids and 1 lignan. The results highlighted the great number of phenolic compounds recovered from filter cake with these techniques, being even higher than the reported content in EVOO and other byproducts. The combination of PLE and freeze-drying resulted in being the best procedure for the recovery of phenolic compounds from filter cake byproduct.

Sofosbuvir is one of the new direct-acting antiviral drugs against hepatitis C virus (HCV) infection. This drug has recently been launched into the market, and generic versions of the medication are expected to be produced by local drug producers in some countries. Therefore, new methods are required to control sofosbuvir in pharmaceuticals. In the present study, a new method based on reversed phase (RP)-ultra-high performance liquid chromatography (UHPLC) coupled to diode array detection (DAD) and mass spectrometry (MS) was developed to facilitate the qualitative and quantitative analysis of sofosbuvir in film coated tablets. A wavelength of 260 nm was selected to perform a cost-effective quantification and the method showed adequate linearity, with an R2 value of 0.9998, and acceptable values of accuracy (75%–102%) and precision (residual standard deviation

Phenolic compounds in rosemary have shown antiproliferative/cytotoxic activity against colorectal cancer cells. The aim of this work was to study in depth the absorption and metabolism of the compounds present in a rosemary extract. An in-situ perfusion assay was performed in mice, for which samples of gastrointestinal liquid taken at different times and plasma obtained at the end of the experiment were analysed by HPLC-ESI-QTOF-MS. The absorption-rate coefficients showed that flavonoids and diterpenes were highly absorbed compared to triterpenes. Several diterpenes and their metabolites were also bioavailable in plasma, highlighting the higher concentrations of glucuronide metabolites compared to non-metabolised phenolic compounds. The antiproliferative/cytotoxic properties could be attributed to the absorbed diterpenes and metabolites, which could reach the colon through bloodstream. On the other hand, compounds poorly absorbed, such as triterpenes and some diterpenes, could exhibit their bioactivity in the large intestine by a mechanism of direct interaction with the microbiota.

This study was designed to investigate the protective effects of Globularia alypum leaves extract (GE) against the nephrotoxicity provoked by a chronic exposure to deltamethrin (DLM) in rats. High-performance liquid chromatography coupled with electrospray ionization tandem quadrupole–time-of-flight mass spectrometry (HPLC-DAD-ESI-QTOF-MS) analysis revealed the presence of thirty-nine compounds among them globularin was the major compound (9444 mg/100 g of dry matter). Results showed that DLM administration altered the renal functions. Whereas, GE treatment restored the increased plasma creatinine, urea and uric acid levels, reduced the elevated MDA and PC levels, significantly normalized the antioxidant enzyme activities. In addition, histopathologic examination confirmed the deltamethrin damage to the renal tissue and revealed renal connective tissue fibrosis and severe necrosis of the proximal tubules with haemorrhage, which was corrected by GE treatment. Therefore, it was speculated that GE presented a protective effects against deltamethrin induced nephrotoxicity through the action of its bioactive compounds.

Nowadays, the transformation activity of the food industry results in the generation of a huge amount of daily discarded vegetables wastes. One of those undervalued by-products are produced during the post-harvesting and processing process of artichokes. In the present research, the potential of artichokes’ bracts and stalks have been evaluated as a natural source of phenolic compounds which could be used as bioactive food ingredients, among others. In this study, the bioactive composition of those wastes has been evaluated using recent advances in extraction and analytical technologies, concretely, pressurized liquid extraction (PLE) followed by high-performance liquid chromatography (HPLC) coupled to electrospray time-of flight mass spectrometry (ESI-TOF/MS) analysis. To achieve this goal, first, the extraction process was evaluated by a comparative study using GRAS (Generally Recognized As Safe) solvents (mixtures of ethanol and water) at different temperatures (40–200 °C). The second step was to deeply characterize the composition of individual polyphenols by HPLC-ESI-TOF/MS in order to establish a comparison among the different PLE conditions applied to extract the phenolic fraction. The analysis revealed a wide variety of phenolic-composition, mainly phenolic acids and flavonoids. The results also highlighted that high percentages of ethanol and medium-high temperatures pointed out to be useful PLE conditions for recovering this kind of phytochemicals, which could be used in different applications, such as functional food ingredients, cosmetics, or nutraceuticals.

In this study, we determined the phytochemical profile of the Spanish “triguero” asparagus landrace “verde-morado” (Asparagus officinalis L.), a wild traditional landrace, and the improved “triguero” HT-801, together with two commercial green asparagus varieties. For comparison, we used reverse-phase high-performance liquid chromatography coupled with diode array electrospray time-of-flight mass spectrometry (RP-HPLC-DAD-ESI-TOF/MS) followed by a permutation test applied using a resampling methodology valid under a relaxed set of assumptions, such as i.i.d. errors (not necessarily normal) that are exchangeable under the null hypothesis. As a result, we postulate that “triguero” varieties (the improved HT-801 followed by its parent “verde-morado”) have a significantly different phytochemical profile from that of the other two commercial hybrid green varieties. In particular, we found compounds specific to the “triguero” varieties, such as feruloylhexosylhexose isomers, or isorhamnetin-3-O-glucoside, which was found only in the “triguero” variety HT-801. Although studies relating the phytochemical content of “triguero” asparagus varieties to its health-promoting effects are required, this characteristic phytochemical profile can be used for differentiating and revalorizating these asparagus cultivars.

The approaches based on high-resolution analytical techniques, such as nuclear magnetic resonance or mass spectrometry coupled to chromatographic techniques, have a determining role in several of the stages necessary for the development of functional foods. The analyses of botanical extracts rich in bioactive compounds is one of the fundamental steps in order to identify and quantify their phytochemical composition. However, the compounds characterized in the extracts are not always responsible for the bioactive properties because they generally undergo metabolic reactions before reaching the therapeutic targets. For this reason, analytical techniques are also applied to analyze biological samples to know the bioavailability, pharmacokinetics and/or metabolism of the compounds ingested by animal or human models in nutritional intervention studies. In addition, these studies have also been applied to determine changes of endogenous metabolites caused by prolonged intake of compounds with bioactive potential. This review aims to describe the main types and modes of application of high-resolution analytical techniques in all these steps for functional food development.

Sesame (Sesamum indicum L.) is a global oil crop. Sesame oil has been regarded as functional oil with antioxidant properties in several in vivo studies but little is known about its minor fraction. In this line, this study figures out the profile of the polar fraction of Egyptian cultivar Giza 32 sesame oil (SG32 oil) employing reversed-phase high-performance liquid chromatography coupled with diode array detection and electrospray ionization-quadrupole-time-of-flight-mass spectrometry and tandem MS. The characterization of the sesame oil metabolites depended on the observation of their retention time values, accurate MS, and MS/MS data, with UV spectra, and compared with relevant literature and available standards. Remarkably, 86 metabolites were characterized and sub-grouped into phenolic acids, lignans, flavonoids, nitrogenous compounds, and organic acids. From the characterized metabolites, 72 compounds were previously characterized in SG32 cake, which presented antioxidant properties, and hence it could contribute to SG32 oil antioxidant properties. Further studies are required to state the presence of such phenolics in commercial sesame oils and what of these compounds resist oil refining.

Nowadays there are evidences from several studies which have revealed the protective effects of food against chronic diseases. These healthy properties have been related to bioactive compounds. Among bioactive substances, the scientific interest in phenolic compounds has stimulated multidisciplinary research on the composition of plant phenolic compounds. The aim of this work has been to determine the bioactive composition of Carao tree seeds (Cassia grandis) and to optimize the recovering of these compounds for developing functional ingredients. To achieve this goal, pressurized liquid extraction (PLE) has been applied to recover these phytochemicals. The optimization of this innovative extraction procedure was performed by a response surface methodology (RSM) based on a central composite design 23 model to address the bioactive compounds extraction. Phenolic compounds recovered by PLE were characterized using reversed-phase high-performance liquid chromatography coupled to electrospray ionization time-of-flight mass spectrometry (HPLC-ESI-TOF-MS). Analytical characterization allowed the identification and quantitation of phenolic compounds belonging to hydroxybenzoic acids and flavonoids (flavonols, flavanols, flavanones and proanthocyanidins). Phytochemical concentrations were used as response variable in order to get the best extraction conditions. These results pointed out that Carao tree seeds can be a potential source of bioactive compounds and PLE extracts could be used as functional ingredients.

Phenolic compounds have shown to have a high bioactive potential against various pathologies, postulating as an interesting alternative to manage some diseases. In this sense, both Lippia citriodora and Hibiscus sabdariffa are two botanical sources with a demonstrated high bioactive potential, in which their antioxidant capacity stands out. In this work, the optimization of the extraction conditions for the recovery of phytochemicals from L. citriodora leaves and H. sabdariffa calyces has been carried out using Response Surface Methodologies (RSM) considering their total polar compounds measured by HPLC-ESI-TOF/MS and Folin-Ciocalteu assay, and its antioxidant capacity evaluated by Ferric Reducing Antioxidant Power (FRAP) and Trolox Equivalent Antioxidant Capacity (TEAC) assays. The results showed that to maximize the antioxidant capacity in H. sabdariffa, a moderate temperature and high ethanol percentage are needed, while a low temperature and a high percentage of ethanol are needed in L. citriodora. In addition, with the results obtained in the multiple response analysis, it is possible to affirm the importance of this type of analysis to develop functional ingredients, taking into account both total content of phenolic compounds and their bioactivity. Furthermore, as confirmed in this study, these analyses can be extrapolated in different techniques and in different matrices, with phenolic compounds from different families being important to develop new high added value products for food, pharmaceutical or cosmetic industries.