A new HS-SPME-GC-MS analytical method to identify and quantify compounds responsible for changes in the volatile profile in five types of meat products during aerobic storage at 4 °C.

Nowadays, it is important to monitor the freshness of meat during storage to protect consumers' health. Volatile organic compounds (VOCs) are responsible for odour and taste of food, and they give an indication about meat quality and freshness. This study had the aim to seek and select potential new markers of meat spoilage through a semi-quantitative analysis in five types of meat (beef, raw and baked ham, pork sausage and chicken) and then to develop a new quantitative analytical method to detect and quantify potential markers on five types of meat simultaneously. Firstly, a new headspace-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) method was developed to evaluate the volatile profile of five types of meat, preserved at 4 °C for 5 days. Among the 40 compounds identified, 15 were chosen and selected as potential shelf-life markers on the basis of their presence in most of meat samples or/and for their constant increasing/decreasing trend within the sample. Afterwards, a quantitative HS-SPME-GC-MS analytical method was developed to confirm which VOCs can be considered markers of shelf-life for these meat products, stored at 4 °C for 12 days. Some of the compounds analyzed attracted attention as they can be considered markers of shelf-life for at least 4 types of meat: 1-butanol, 3-methylbutanol, 1-hexanol, 2-nonanone, nonanal, 1-octen-3-ol and linalool. In conclusion, in this study a new quantitative HS-SPME-GC-MS analytical method to quantity 15 VOCs in five types of meat was developed and it was demonstrated that some of the compounds quantified can be considered markers of shelf-life for some of the meat products analyzed.

Use of grape by-products in aquaculture: New frontiers for a circular economy application.

Grape by-products have already been used in cosmetics, food industries, but also animal feed industry, especially monogastrics and in aquaculture. Grape by-products have been studied for a long time and their principal activities are antimicrobial and antioxidant. Concerning aquaculture, the great demand and necessity to replace animal sources with vegetable ones, has placed grape by-products as possible new phytonutrients with beneficial properties. The purpose of this review is to describe the use of grape by-products in aquaculture, during the last decade, concerning their effects on: 1) gut health and welfare status; 2) growth performances; 3) quality of fillets and flesh during the rearing cycle and shelf-life products. Although other studies highlighted that the high supplementation of grape by-products could negatively affect fish health and growth, due to antinutritional factors (tannins), grape by-products are proven to be valuable phytonutrients that can be incorporated into fish feed to enhance growth and health during rearing conditions. Even in fish products, their utilization has proven to elongate the properties and shelf-life of fillets and minces. Further studies to evaluate the possible integrations or replacements with grape by-products in fish feed in order to evaluate their effectiveness in aquaculture from a sustainable circular economy perspective will be desirable to enhance the use of these products.

Effect of Brewing Methods on Acrylamide Content and Antioxidant Activity: Studying Eight Different Filter Coffee Preparations.

The aim of this study was to investigate the parameters affecting the extraction of positive molecules such as chlorogenic acids and antioxidants, as well as potentially carcinogenic substances such as acrylamide, in different coffee brewing methods. Three coffee varieties, each assigned a different roasting degree, were used to prepare coffee brews following eight different preparation methods. Acrylamide was quantified using the HPLC-MS/MS instrument, while chlorogenic acids and caffeine were quantified using the HPLC-DAD system. Three spectrophotometric analyses were also performed (DPPH, TFC and TPC) to evaluate antioxidant activity. The results showed that the main brewing parameters, which have the greatest influence on the final content of these compounds, were the volume of water used, more specifically the brewing ratio (coffee to water ratio), the extraction time and the particle size of the coffee powder. In addition, the variables that have the greatest impact on the discrimination of the preparation methods studied are total chlorogenic acid content, TFC, TPC, caffeine and the DPPH assay. For this reason, the recipe and infusion parameters used for each of the extraction systems are the key factors that determine the extraction of coffee components and, consequently, the quality of the cup.

Discrimination of Filter Coffee Extraction Methods of a Medium Roasted Specialty Coffee Based on Volatile Profiles and Sensorial Traits.

An untargeted gas chromatography-mass spectrometry (GC-MS) approach combined with sensory analysis was used to present the effects of different extraction methods (i.e., Pure Brew, V60, AeroPress, and French Press) on specialty graded Coffea arabica from Kenya. Partial Least Square Discriminant analysis and hierarchical clustering were applied as multivariate statistical tools in data analysis. The results showed good discrimination and a clear clustering of the groups of samples based on their volatile profiles. Similarities were found related to the filter material and shape used for the extraction. Samples extracted with paper filters (V60 and AeroPress) resulted in higher percentages of caramel-, and flowery-related compounds, while from metal filter samples (Pure Brew and French Press), more fruity and roasted coffees were obtained. Discriminant analysis allowed the identification of eight compounds with a high VIP (variable important in projection) discriminant value (i.e., >1), with 2-furanmethanol being the main feature in discrimination. Sensorial analyses were carried out through an expert panel test. The main evaluations revealed the French Press system as the lowest-scored sample in all the evaluated parameters, except for acidity, where its score was similar to V60. In conclusion, the data obtained from GC-MS analyses were in line with the sensorial results, confirming that the extraction process plays a fundamental role in the flavor profile of filter coffee beverages.

Inulin Functionalized "Giuncata" Cheese as a Source of Prebiotic Fibers.

The development of functional foods in the dairy sector represents a flourishing field of technological research. In this study, an Italian fresh cheese as "giuncata" was enriched with inulin, a dietary fiber, with the aim of developing a product with improved nutritional properties in terms of prebiotic action on intestinal microbiota. An inulin concentration of ~4% w/w was determined in the fresh cheese after the fortification process, enabling the claim of being a "source of dietary fiber" (inulin > 3 g/100 g) according to the European regulation. The addition of inulin has no effect on the pH of cheese and does not relevantly influence its color as well as the total fat content (fat reduction ~0.61%) in comparison to the control. Mechanical properties of the cheese were also not markedly affected as evidenced from rheological and tensile testing analyses. Indeed, the incorporation of inulin in "giuncata" only exerts a slight "softening effect" resulting in a slightly lower consistency and mechanical resistance in comparison to the control. Overall, this study demonstrates the feasibility of producing a fiber-enriched dairy functional food from a large consumed fresh and soft cheese as "giuncata".

Volatile Profile of Strawberry Fruits and Influence of Different Drying Methods on Their Aroma and Flavor: A Review.

Strawberries are the most popular berry fruit in the world, due to their distinctive aroma, flavor, and known health properties. Because volatile substances play a large role in strawberry flavor, even little alterations can have a big impact on how the fruit tastes. Strawberries are thought to have a complex aroma. Fresh strawberry fruits contain more than 360 volatile compounds, including esters, furans, terpenes, alcohols, aldehydes, ketones, and sulfur compounds. Despite having far lower concentrations than esters, terpenoids, furanones, and sulfur compounds, all have a considerable impact on how people perceive the aroma of strawberries. With a focus on the active aroma components and the many analytical methods used to identify them, including gas chromatography, electronic nose sensing, and proton-transfer- reaction mass spectrometry, the present review's aim was to provide a summary of the relevant literature. Additionally, strawberry fruits are frequently dried to create a powder in order to increase their shelf life. Consequently, the impact of various drying techniques on strawberries' volatile profile was investigated in the current review. This review can be considered a good reference for research concerning the aroma profile of strawberries. It helps to better understand the complex aroma and flavor of strawberries and provides a guide for the effects of drying processing.

Development of Innovative Vitamin D Enrichment Designs for Two Typical Italian Fresh Cheeses: Burrata and Giuncata.

The aim of this research was to develop innovative cheeses fortified with vitamin D3 (VD3). Formulation studies and analyses of textural properties and chemicals were carried out for these developments. Two traditional Italian varieties of cheese (giuncata and burrata) were studied. For giuncata, the fortification of milk for cheese production provided a VD3 retention level of 43.9 ± 0.6% in the food matrix. For burrata, the VD3 ingredient was incorporated into the creamy inner part after mixing, maintaining the textural quality of the product (adhesiveness 4.3 ± 0.4 J × 10-3; firmness 0.7 ± 0.0 N; and cohesiveness 0.8 ± 0.2). The optimized enrichment designs allowed to obtain homogenous contents of VD3 during the production of giuncata (0.48 ± 0.01 µg/g) and burrata cheeses (0.32 ± 0.02 µg/g). Moreover, analyses revealed the high stability of VD3 during the storage of the two fortified cheese types (2 weeks, 4 °C). These fortification designs could be implemented at an industrial scale to obtain new cheese types enriched in VD3 and thus contribute to the reduction in VD deficiency prevalence.

Polyphenols, Saponins and Phytosterols in Lentils and Their Health Benefits: An Overview.

The lentil (Lens culinaris L.) is one of the most important legumes (family, Fabaceae). It is a natural functional food rich in many bioactive compounds, such as polyphenols, saponins and phytosterols. Several studies have demonstrated that the consumption of lentils is potentially important in reducing the incidence of a number of chronic diseases, due to their bioactive compounds. The most common polyphenols in lentils include phenolic acids, flavan-3-ol, flavonols, anthocyanidins, proanthocyanidins or condensed tannins, and anthocyanins, which play an important role in the prevention of several degenerative diseases in humans, due to their antioxidant activity. Furthermore, lentil polyphenols are reported to have antidiabetic, cardioprotective and anticancer activities. Lentil saponins are triterpene glycosides, mainly soyasaponins I and ßg. These saponins have a plasma cholesterol-lowering effect in humans and are important in reducing the risk of many chronic diseases. Moreover, high levels of phytosterols have been reported in lentils, especially in the seed coat, and ß-sitosterol, campesterol, and stigmasterol are the most abundant. Beyond their hypocholesterolemic effect, phytosterols in lentils are known for their anti-inflammatory activity. In this review, the current information on the nutritional composition, bioactive compounds including polyphenols, saponins and phytosterols, and their associated health-promoting effects are discussed.

A New HPLC-MS/MS Method for the Simultaneous Determination of Quercetin and Its Derivatives in Green Coffee Beans.

Green coffee (Coffee arabica and Coffee robusta) is one of the most commonly traded goods globally. Their beans are enriched with polyphenols and numerous health benefits are associated with their consumption. The main aim of this work was to develop a new and fast analytical HPLC-MS/MS method to simultaneously determine six flavonoid polyphenolic compounds (quercetin, rutin, isorhamnetin, quercetin-3-glucouronide, hyperoside, and quercitrin) in 22 green coffee samples from six different geographical origins (Ethiopia, Brazil, Guatemala, Nicaragua, India and Colombia). In addition, by adjusting pH, temperature, solvent type, and extraction duration, several extraction methods such as acidic and alkaline hydrolysis, and extraction without hydrolysis were evaluated. The optimal extraction procedure in terms of recovery percentages (78.67-94.09%)was acidic hydrolysis at pH 2, extraction temperature of 60 °C, extraction solvent of 70% ethanol, and extraction duration of 1.5 h. Hyperoside (878-75 µg/kg) was the most abundant compound followed by quercitrin (408-38 µg/kg), quercetin (300-36 µg/kg), rutin (238-21 µg/kg), and quercetin-3-glucouronide (225-7 µg/kg), while isorhamnetin (34-3 µg/kg) showed the lowest amount. Overall, green coffee beans are rich in flavonoid polyphenolic compounds and could be used as part of a healthy diet.

Optimization of Solvent-Free Microwave-Assisted Hydrodiffusion and Gravity Extraction of Morus nigra L. Fruits Maximizing Polyphenols, Sugar Content, and Biological Activities Using Central Composite Design.

Black mulberry, Morus nigra L. (family: Moraceae), is a healthy food and medicinal plant. Microwave hydrodiffusion and gravity (MHG) is one of the most innovative applications of solvent-free microwave extraction. The aim of this study was to optimize for the first time the MHG solvent-free extraction of polyphenols and sugars from M. nigra fruits. Optimization was carried out using a central composite design (CCD) with selected responses such as extraction yield, total polyphenol (TPC), flavonoid (TFC), anthocyanin (TAC), and sugar (TSC) contents, in addition to DPPH radical scavenging, and α-glucosidase (AGHi), lipase (Li), and xanthine oxidase (XOi) inhibition as tools to evaluate the best parameters for efficient and rapid extraction of black mulberry. The optimized extract was characterized in terms of the aforementioned parameters to validate the models, and was further analyzed for 36 individual polyphenols using HPLC-MS/MS. The optimized MHG extract was finally compared with traditional extracts, and demonstrated much better performance in terms of TPC, TAC, and Li, while the traditional extracts showed better XOi and AGHi. In conclusion, MHG is a valuable green technique for the production of non-degraded black mulberry polyphenol-rich extract and we suggest its larger use in the pharmaceutical and food industries.

Coffee silverskin: Characterization of B-vitamins, macronutrients, minerals and phytosterols.

The present study assessed the nutritional composition of coffee silverskin (CSS) obtained from arabica roasted coffee. Following validated analytical methods, CSS resulted to be a high source of proteins (14.2 g/100 g) and dietary fibers (51.5 g/100 g). Moreover, the mineral analysis revealed high contents of calcium (1.1 g/100 g) and potassium (1.0 g/100 g). To date, this study provided the widest mineral profile of CSS with 30 minerals targeted including 23 microminerals with high levels of iron (238.0 mg/kg), manganese (46.7 mg/kg), copper (37.9 mg/kg), and zinc (31.9 mg/kg). Moreover, vitamins B2 (0.18-0.2 mg/kg) and B3 (2.5-3.1 mg/kg) were studied and reported for the first time in CSS. ß-sitosterol (77.1 mg/kg), campesterol, stigmasterol, and Δ5-avenasterol, were also observed from the phytosterol analysis of CSS with a total level of 98.4 mg/kg. This rich nutritional profile highlights the potential values of CSS for innovative reuses in bioactive ingredients development.

A new HPLC-MS/MS method for the simultaneous determination of 36 polyphenols in blueberry, strawberry and their commercial products and determination of antioxidant activity.

Berry fruits consumption has increased in recent years because they are rich sources of polyphenols with reported health benefits. The aim of the present work was to develop a new comprehensive and fast HPLC-MS/MS method for simultaneous determination of 36 phenolic compounds (7 anthocyanins, 9 flavonols, 4 flavan-3-ols, 2 dihydrochalcones, 2 flavanones and 12 phenolic acids) present in blueberry, strawberry, and their fruit jam. Blueberry fruits showed higher contents of anthocyanins, flavonols and phenolic acids, while strawberry fruits exhibited higher contents of flavan-3-ols, dihydrochalcones and flavanones. Anthocyanins were the main phenolic constituents in both berries. Furthermore, the higher total phenolic content in the blueberry fruit and jam justified their greater antioxidant capacity measured by DPPH free radical assay, compared to strawberry. In conclusion, this new HPLC-MS/MS method is useful and reliable for quality control and authentication analyses of blueberry and strawberry fruits and their commercial food products, such as jams.

The Impact of Plasma Activated Water Treatment on the Phenolic Profile, Vitamins Content, Antioxidant and Enzymatic Activities of Rocket-Salad Leaves.

Plasma activated water (PAW) recently received much attention as an alternative food preservation method. However, its effects on food quality are still scarce. This study evaluates the effect of PAW processing time on bioactive compounds of rocket-salad leaves including: 18 phenolic compounds, vitamin C, riboflavin, nicotinic acid, and nicotinamide. Moreover, the impact of PAW on both antioxidant (DPPH) and peroxidase (POD) activities was also investigated. This was performed using HPLC-DAD, HPLC-MS/MS, and spectrophotometric analysis. All treatments induced non-significant increases in total phenolic contents. However, depending on processing time, significant increases or decreases of individual phenolic compounds were observed. PAW-10 and -20 increased the ascorbic acid content to 382.76 and 363.14 mg/100 g, respectively, compared to control (337.73 mg/100 g). Riboflavin and nicotinic acid contents were increased significantly in PAW-20 (0.53 and 1.26 mg/100), compared to control (0.32 and 0.61 mg/100 g, respectively). However, nicotinamide showed non-significant increase in all treatments. Antioxidant activity improved significantly only in PAW-20, while peroxidase activity was reduced up to 36% in the longest treatment. In conclusion, PAW treatment could be an effective technique for rocket decontamination since it positively influenced the quality of rocket, improving the retention of polyphenols and vitamins.

Effect of Plasma Activated Water on Selected Chemical Compounds of Rocket-Salad (Eruca sativa Mill.) Leaves.

Plasma activated water (PAW) has proven to be a promising alternative for the decontamination of rocket leaves. The impact of PAW on the volatile profile, phytosterols, and pigment content of rocket leaves was studied. Leaves were treated by PAW at different times (2, 5, 10, and 20 min). Compounds of the headspace were detected and quantified using GC-MS analysis. A total of 52 volatile organic compounds of different chemical classes were identified. Glucosinolate hydrolysis products are the major chemical class. PAW application induced some chemical modifications in the volatile compounds. Changes in the content of the major compounds varied with the increase or decrease in the treatment time. However, PAW-10 and -2 were grouped closely to the control. A significant decrease in the content of ß-sitosterol and campesterol was observed after PAW treatment, except for PAW-10, which showed a non-significant reduction in both compounds. A significant increase in ß carotene, luteolin, and chlorophyll b was observed after the shortest treatment time of PAW-2. A reduction in chlorophyll content was also observed, which is significant only at longer treatment, or PAW-20. Overall, PAW has proven to be a safe alternative for rocket decontamination.

Effect of Roasting, Boiling, and Frying Processing on 29 Polyphenolics and Antioxidant Activity in Seeds and Shells of Sweet Chestnut (Castanea sativa Mill.).

Sweet chestnuts (Castanea sativa Mill.) are highly prized nuts, and the consumption of fresh chestnuts is usually preceded by roasting, boiling, and frying. The aim of this work was to simultaneously analyze 29 polyphenolic compounds for the first time in raw, boiled, roasted, and fried chestnut seeds and shells using HPLC-MS/MS. Principal component analysis depending on the HPLC-MS/MS results showed that roasting, boiling, and frying affected the contents of 25 detected phenolic compounds in a unique way, of which the most notable phenolics were gallic acid, ellagic acid, and (+)-catechin. Additionally, total polyphenolic content (TPC) was measured via the Folin-Ciocalteu method, and TPC in seeds and inner and outer shells was increased in all treatments except for microwave-roasted seeds. Furthermore, the higher TPC in the inner and outer shells when compared to seeds supported their higher antioxidant activity (AOA) determined via the DPPH experiment. AOA of seeds was increased in all treatments, while the AOA of shells was higher in roasting and lower in boiling and frying treatments. The assessment of these changes is necessary so that chestnut seed consumption and the recycling of their shells as a natural source of antioxidants can be maximized.

Characterization of the Aroma Profile and Main Key Odorants of Espresso Coffee.

Espresso coffee (EC) is a common coffee preparation technique that nowadays is broadly widespread all over the globe. Its popularity is in part attributed to the intense aroma and pleasant flavor. Many researchers have studied and reviewed the aroma of the coffee, but there is a lack of specific review focused on EC aroma profile even if it is intensively investigated. Thus, the objective of the current review was to summarize the aroma profile of EC and how different preparation variables can affect EC flavor. Moreover, a collection of diverse analytical procedures for volatile analysis was also reported. The findings of this survey showed that the volatile fraction of EC is extremely complex, but just some compounds are responsible for the characteristic aroma of the coffee, such as some aldehyde, ketones, furanones, furans, sulfur compounds, pyrazines, etc. In addition, during preparation, some variables, e.g., temperature and pressure of water, granulometry of the coffee particle, and brew ratio, can also modify the aroma profile of this beverage, and therefore its quality. A better understanding of the aroma fraction of EC and how the preparation variables should be adjusted according to desired EC would assist coffee workers in obtaining a higher quality product.

Influence of Freezing and Different Drying Methods on Volatile Profiles of Strawberry and Analysis of Volatile Compounds of Strawberry Commercial Jams.

Strawberry is the most consumed berry fruit worldwide due to its unique aroma and flavor. Drying fruits to produce a powder represents one of the possible conservation methods to extend their shelf-life. The aim of the present study was to compare the influence of freezing and different drying methods on the volatile profile of strawberry using the HS-SPME/GC-MS method, in addition to analysis of strawberry jam volatiles. A total of 165 compounds were identified, accounting for 85.03-96.88% of the total volatile compositions. Results and PCA showed that freezing and each drying process affected the volatile profile in a different way, and the most remarkable representative differential volatiles were ethyl hexanoate, hexyl acetate, (E)-2-hexenyl acetate, mesifurane, (E)-nerolidol, γ-decalactone, 1-hexanol, and acetoin. Shade air-dried, frozen, freeze-dried, and oven-dried 45 °C samples retained more of the fruity and sweet aromas of strawberry, representing more than 68% of the total aroma intensity according to the literature. In contrast, the microwave-drying method showed drastic loss of fruity esters. Strawberry jams demonstrated complete destruction of esters and alcohols in most jams, while terpenes were significantly increased. These findings help better understand the aroma of strawberry and provide a guide for the effects of drying, freezing, and jam processing.

Quantification of 17 Endogenous and Exogenous Steroidal Hormones in Equine and Bovine Blood for Doping Control with UHPLC-MS/MS.

A simple and fast analytical method able to simultaneously identify and quantify 17 endogenous and exogenous steroidal hormones was developed in bovine and equine blood using UHPLC-MS/MS. A total amount of 500 µL of sample was deproteinized with 500 µL of a mixture of methanol and zinc sulfate and evaporated. The mixture was reconstituted with 50 µL of a solution of 25% methanol and injected in the UHPLC-MS/MS triple quadrupole. The correlation coefficients of the calibration curves of the analyzed compounds were in the range of 0.9932-0.9999, and the limits of detection and quantification were in the range of 0.023-1.833 and 0.069-5.5 ppb, respectively. The developed method showed a high sensitivity and qualitative aspects allowing the detection and quantification of all steroids in equine and bovine blood. Moreover, the detection limit of testosterone (50 ppt) is half of the threshold admitted in plasma (100 ppt). Once validated, the method was used to quantify 17 steroid hormones in both bovine and equine blood samples. The primary endogenous compounds detected were corticosterone (range 0.28-0.60 ppb) and cortisol (range 0.44-10.00 ppb), followed by androstenedione, testosterone and 11-deoxycortisol.

Development of functional whey cheese enriched in vitamin D3: nutritional composition, fortification, analysis, and stability study during cheese processing and storage.

"Ricotta" cheese is a traditional and popular Italian fresh whey cheese commonly produced from cow's milk. Food fortification is an efficient strategy to reduce the high global prevalence of vitamin D deficiency. This study aims to study the chemical-nutritional analysis of ricotta cheese and to assess its suitability as a dairy matrix for vitamin D fortification. The chemical-nutritional analyses revealed that ricotta cheese is a good source of proteins (7.8 g/100 g) with high levels of branched-chain amino acids (1.8 g/100 g). Moreover, ricotta contains high levels of calcium (0.4 g/100 g) and phosphorus (0.2 g/100 g). 50 mg of vitamin D3 were added to 95 kg of cheese reaching a mean fortification level of 41.4 ± 4.0 µg/100 g of ricotta cheese. The fortification study showed that vitamin D homogenously distributes in ricotta cheese after the homogenisation process. Moreover, vitamin D3 has high heat stability (93.8 ± 1.8%) and remains stable throughout the shelf-life of the fortified food. This study demonstrates that ricotta cheese represents an ideal alternative dairy matrix for vitamin D3 fortification.

Acrylamide formation and antioxidant activity in coffee during roasting - A systematic study.

The aim of this study was to investigate the effect of the coffee roasting process on both toxic and some beneficial antioxidant compounds, applying a systematic and broad approach. Arabica and Robusta green coffee beans were roasted in a lab-scale roaster for different times in order to achieve five roasting degrees (from light to dark) and to assess the evolution of acrylamide (AA), trigonelline, nicotinic acid and caffeoylquinic acids contents (determined by HPLC) as well as antioxidant activity (evaluated by Folin-Ciocalteu, FRAP, DPPH, ABTS assays). The results confirmed that the AA levels and antioxidant activity reached a maximum in the first coffee roasting degrees and then decreased prolonging the heating process, both in Arabica and Robusta samples. Nevertheless, the thermal reduction observed was greater for AA compared to antioxidant activity, which was only slightly reduced due to the balance between the degradation and the neoformation of antioxidant compounds.