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1.
Chem Biodivers ; 21(2): e202301629, 2024 Feb.
Article in English | MEDLINE | ID: mdl-38109266

ABSTRACT

Three Portuguese olive oils with PDO ('Azeite do Alentejo Interior', 'Azeites da Beira Interior' and 'Azeite de Trás-os-Montes') were studied considering their physicochemical quality, antioxidant capacity, oxidative stability, total phenols content, gustatory sensory sensations and Fourier transform infrared (FTIR) spectra. All oils fulfilled the legal thresholds of EVOOs and the PDO's specifications. Olive oils from 'Azeite da Beira Interior' and 'Azeite de Trás-os-Montes' showed greater total phenols contents and antioxidant capacities, while 'Azeites da Beira Interior' presented higher oxidative stabilities. Linear discriminant models were developed using FTIR spectra (transmittance and the 1st and 2nd derivatives), allowing the correct identification of the oils' PDO (100 % sensitivity and specificity, repeated K-fold-CV). This study also revealed that multiple linear regression models, based on FTIR transmittance data, could predict the sweet, bitter, and pungent intensities of the PDO oils (R2 ≥0.979±0.016; RMSE≤0.26±0.05, repeated K-fold-CV). This demonstrates the potential of using FTIR as a non-destructive technique for authenticating oils with PDO.


Subject(s)
Antioxidants , Phenols , Olive Oil/chemistry , Spectroscopy, Fourier Transform Infrared , Fourier Analysis , Portugal , Phenols/analysis , Plant Oils/chemistry
2.
Food Chem ; 398: 133945, 2023 Jan 01.
Article in English | MEDLINE | ID: mdl-35986990

ABSTRACT

Olive oils from seven Portuguese regions were selected to study the effect of the geographical origin on the oils' composition. Quality parameters, fatty acids, tocopherols, hydroxytyrosol and tyrosol derivatives, and oxidative stability were evaluated. All olive oils could be classified as extra virgin, and the geographical origin significantly affected the oils chemical composition. Principal component analysis further confirmed the significant impact of the geographical origin on the composition and, indirectly, on stability of the oils, showing that the evaluated parameters could be used as markers for geographical origin identification. Alternatively, Fourier transform infrared spectroscopy was applied, allowing to establish a linear discriminant model that correctly identified the geographical origin of the olive oils with a mean sensitivity of 99 ± 3 % (internal validation), confirming the impact of the oil origin on its characteristics. This finding allowed foreseeing the future application of the spectroscopy approach as a green, fast and non-invasive authentication tool.


Subject(s)
Galega , Fatty Acids/analysis , Olive Oil/chemistry , Plant Oils/chemistry , Spectroscopy, Fourier Transform Infrared , Tocopherols/chemistry
3.
Sensors (Basel) ; 22(24)2022 Dec 09.
Article in English | MEDLINE | ID: mdl-36560020

ABSTRACT

The geographical traceability of extra virgin olive oils (EVOO) is of paramount importance for oil chain actors and consumers. Oils produced in two adjacent Portuguese regions, Côa (36 oils) and Douro (31 oils), were evaluated and fulfilled the European legal thresholds for EVOO categorization. Compared to the Douro region, oils from Côa had higher total phenol contents (505 versus 279 mg GAE/kg) and greater oxidative stabilities (17.5 versus 10.6 h). The majority of Côa oils were fruity-green, bitter, and pungent oils. Conversely, Douro oils exhibited a more intense fruity-ripe and sweet sensation. Accordingly, different volatiles were detected, belonging to eight chemical families, from which aldehydes were the most abundant. Additionally, all oils were evaluated using a lab-made electronic nose, with metal oxide semiconductor sensors. The electrical fingerprints, together with principal component analysis, enabled the unsupervised recognition of the oils' geographical origin, and their successful supervised linear discrimination (sensitivity of 98.5% and specificity of 98.4%; internal validation). The E-nose also quantified the contents of the two main volatile chemical classes (alcohols and aldehydes) and of the total volatiles content, for the studied olive oils split by geographical origin, using multivariate linear regression models (0.981 ≤ R2 ≤ 0.998 and 0.40 ≤ RMSE ≤ 2.79 mg/kg oil; internal validation). The E-nose-MOS was shown to be a fast, green, non-invasive and cost-effective tool for authenticating the geographical origin of the studied olive oils and to estimate the contents of the most abundant chemical classes of volatiles.


Subject(s)
Electronic Nose , Taste , Humans , Olive Oil/chemistry , Portugal , Aldehydes
4.
Pharmaceuticals (Basel) ; 15(11)2022 Oct 27.
Article in English | MEDLINE | ID: mdl-36355503

ABSTRACT

Designing oral formulations for children is very challenging, especially considering their peculiarities and preferences. The choice of excipients, dosing volume and palatability are key issues of pediatric oral liquid medicines. The purpose of the present study is to develop an oral pediatric solution of a model bitter drug (ranitidine) following a patient centric design process which includes the definition of a target product profile (TPP). To conclude on the matching of the developed solution to TPP, its chemical and microbiological stability was analyzed over 30 days (stored at 4 °C and room temperature). Simulation of use was accomplished by removing a sample with a syringe every day. Taste masking was assessed by an electronic tongue. The developed formulation relied on a simple taste masking strategy consisting in a mixture of sweeteners (sodium saccharine and aspartame) and 0.1% sodium chloride, which allowed a higher bitterness masking effectiveness in comparison with simple syrup. The ranitidine solution was stable for 30 days stored at 4 °C. However, differences were noted between the stability protocols (unopened recipient and in-use stability) showing the contribution of the simulation of use to the formation of degradation products. Stock solution was subjected to acid and alkali hydrolysis, chemical oxidation, heat degradation and a photo degradation stability assessment. The developed pediatric solution matched the TPP in all dimensions, namely composition suitable for children, preparation and handling adapted to hospital pharmaceutical compounding and adequate stability and quality. According to the results, in-use stability protocols should be preferred in the stability evaluation of pediatric formulations.

5.
Int J Food Sci ; 2022: 9189575, 2022.
Article in English | MEDLINE | ID: mdl-35898417

ABSTRACT

The nutraceutical properties of Punica granatum L. are not restricted to the edible portion of the fruit but also to the peels and seeds, flowers, leaves, and tree bark. The recovery and valorization of the peel and seeds (ca. 50% of the whole fruit), besides the positive environmental impact, can be viewed as a source of natural bioactive compounds. Thus, the bioactive properties of extracts of pomegranate peel and seeds from Acco and Wonderful known cultivars, as well as of the novel Big Full cultivar, were evaluated. The dried and ground pomegranate by-products were submitted to a conventional solid/liquid extraction with ethanol/water mixtures (0%, 25%, 50%, and 75% of EtOH, v/v). The obtained extracts were characterized in terms of total phenolic compounds (TPC), total flavonoids (TF), and antioxidant activity (AA), determined by the DPPH radical scavenging activity and expressed as IC50 (half maximum inhibitory concentration). With the exception of the Acco cultivar, the extraction yield (EY) was higher for peels, whose extracts showed higher TPC, TF, and IC50 (lower AA). The extracts obtained from the by-products of the Big Full cultivar had a statistically higher overall bioactive potential (TPC: 0.36 mg GAE/mg extract; TF: 0.031 mg CATE/mg extract; IC50: 0.51 mg/mL) compared to the other two studied cultivars. Furthermore, the EY was enhanced by solvents richer in ethanol (50-75%), allowing obtaining extracts richer in TPC and TF with higher AA. Finally, it was shown that EY combined with bioactive data allowed a satisfactory principal component unsupervised differentiation of the pomegranate extracts according to the type of by-product used.

6.
Food Chem ; 395: 133570, 2022 Nov 30.
Article in English | MEDLINE | ID: mdl-35777205

ABSTRACT

At olive oil industrial extraction, water addition is a practice overcoming the formation of thick pastes. The effect of water addition (0 to 6.2%, kgadded water/kgolives), during the industrial milling of cv. Arbequina olives, on the oils' chemical-sensory quality, was evaluated. Despite the extra virgin olive oil classification, compared with the water incorporation (1.2-6.2%), extraction without water addition resulted into oils that showed less primary oxidation (lower peroxide values and K232), greater total phenolic content (+12-22%) and higher oxidative stability (+22-31%). No water addition increased the oils secoiridoids content (+5-13%), mainly oleacein (+27-79%). Oils extracted without water addition had a more intense ripe fruity sensation (≥ +11%) but lower fruit intensities (at least -4%). Thus, the quality and stability of the cv. Arbequina oils can be favoured if extracted without adding water during the olives industrial milling.


Subject(s)
Olea , Plant Oils , Fruit/chemistry , Olive Oil/analysis , Oxidation-Reduction
7.
Food Chem ; 393: 133327, 2022 Nov 01.
Article in English | MEDLINE | ID: mdl-35653996

ABSTRACT

Leaves incorporation during the extraction of olive oils can enhance their chemical-sensory quality. Thus, leaves from cvs. Arbequina or Santulhana were added (1%, w/w) during the extraction of Arbequina oils using an Abencor system, being discussed the impacts on the phenolics and volatiles formation enzymatic pathways. Leaves addition contributed to a significant decrease (P-value < 0.05) of the contents of secoiridoids (-11%), C6-aldehydes (-16%), and ester compounds (-22%). This could be tentatively related to a reduction of the enzymatic activity of secoiridoids biosynthesis and lipoxygenase pathways, promoted by the leaves' addition. Moreover, in the presence of leaves, the oils' total contents of phenolics and volatiles were significantly reduced (-7 and -17%, respectively). Contrary, the incorporation of leaves significantly increased (P-value < 0.05) the contents of C6-alcohols (+37%) and the intensities of the green fruity (+25%) and apple (+30%) sensations.


Subject(s)
Olea , Volatile Organic Compounds , Iridoids , Olea/metabolism , Olive Oil/analysis , Phenols/analysis , Plant Leaves/chemistry , Plant Oils , Volatile Organic Compounds/metabolism
8.
Foods ; 11(7)2022 Mar 29.
Article in English | MEDLINE | ID: mdl-35407079

ABSTRACT

Pomegranate by-products can be an asset to the food industry due to the richness in bioactive and antimicrobial compounds. This work studied the influence of conventional solvent and sonication-assisted extraction methods on the bioactive profile, antimicrobial properties, and phytotoxicity effect of the peels and seeds extracts from Acco, Big Full, and Wonderful pomegranate cultivars. The bioactive composition of the extracts was evaluated for the content of total phenolics, total flavonoids, and antioxidant activity (expressed as the half-maximal inhibitory concentration-IC50) by spectrophotometric methods, while the tannins were determined by titration and the anthocyanins were estimated by the pH-differential method. For the evaluation of the antimicrobial activity, the disk diffusion method of Kirby-Bauer was adapted through inhibition halos against Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Bacillus cereus, and Yarrowia lipolytica. The extracts' phytotoxicity was evaluated in vitro on garden-cress seeds. Extracts from conventional extraction were richer in total phenolics, expressed as gallic acid equivalents (0.16-0.73 mg GAE/mg extract), while those from sonication-assisted extraction had higher contents of total flavonoids, expressed as catechin equivalents (0.019-0.068 mg CATE/mg extract); anthocyanins, expressed as cyanidin-3-glucoside (0.06-0.60 µg C3G/mg, dry basis); and antioxidant activity (IC50, 0.01-0.20 mg/mL). All extracts were more effective against Gram-positive bacteria and yeasts than Gram-negative bacteria. In general, the sonication-assisted extracts led to higher inhibition halos (8.7 to 11.4 mm). All extracts presented phytotoxicity against garden-cress seeds in the tested concentrations. Only the lowest concentration (0.003 mg/mL) enabled the germination of seeds and root growth, and the sonication-assisted extracts showed the highest Munoo-Liisa vitality index (51.3%). Overall, sonication-assisted extraction obtained extracts with greater bioactive and antimicrobial potential and less phytotoxicity.

9.
Plants (Basel) ; 11(3)2022 Jan 19.
Article in English | MEDLINE | ID: mdl-35161238

ABSTRACT

In inland areas of Portugal and some regions of the Mediterranean basin, olive production is based on traditional olive groves, with low intensification, local cultivars, aged plants, and centenarian trees. These plants play a key role in the ecosystem, contributing to carbon sequestration and possessing a high genetic diversity, particularly important for selecting cultivars more resistant to climatic changes. Appreciation of the value of this genetic diversity implies genetic, morphological, and physicochemical characterization of centenarian trees, which is expensive and time-consuming. Sensory evaluation is also of utmost importance. Thus, in this study, centenarian olive trees were selected in the Côa Valley region, a UNESCO World Heritage site. The descriptive sensory profile of their extracted olive oils was established and used to cluster the oils, using hierarchical clustering analysis, and consequently the olive trees, into five groups with similar intensities of perceived olfactory-gustatory attributes. Each cluster revealed olive oils with unique sensory patterns, presumably due to similarities of the olive trees, confirming the potential of the proposed screening approach. The identification of sensorially homogeneous oil-tree groups would reduce the number of specimens needed for subsequent morphological, genetic, and chemical characterization, allowing a cost-effective and robust future evaluation procedure.

10.
Biosensors (Basel) ; 13(1)2022 Dec 24.
Article in English | MEDLINE | ID: mdl-36671854

ABSTRACT

The detection and level assessment of microorganisms is a practical quality/contamination indicator of food and water samples. Conventional analytical procedures (e.g., culture methods, immunological techniques, and polymerase chain reactions), while accurate and widely used, are time-consuming, costly, and generate a large amount of waste. Electronic noses (E-noses), combined with chemometrics, provide a direct, green, and non-invasive assessment of the volatile fraction without the need for sample pre-treatments. The unique olfactory fingerprint generated during each microorganism's growth can be a vehicle for its detection using gas sensors. A lab-made E-nose, comprising metal oxide semiconductor sensors was applied, to analyze solid medium containing Gram-positive (Enterococcus faecalis and Staphylococcus aureus) or Gram-negative (Escherichia coli and Pseudomonas aeruginosa) bacteria. The electrical-resistance signals generated by the E-nose coupled with linear discriminant analysis allowed the discrimination of the four bacteria (90% of correct classifications for leave-one-out cross-validation). Furthermore, multiple linear regression models were also established allowing quantifying the number of colony-forming units (CFU) (0.9428 ≤ R2 ≤ 0.9946), with maximum root mean square errors lower than 4 CFU. Overall, the E-nose showed to be a powerful qualitative-quantitative device for bacteria preliminary analysis, being envisaged its possible application in solid food matrices.


Subject(s)
Electronic Nose , Nose , Smell , Escherichia coli , Bacteria
11.
Foods ; 10(11)2021 Nov 22.
Article in English | MEDLINE | ID: mdl-34829167

ABSTRACT

Cv. Arbequina extra virgin olive oils (EVOO) were flavored with cinnamon, garlic, and rosemary and characterized. Although flavoring significantly affected the physicochemical quality parameters, all oils fulfilled the legal thresholds for EVOO classification. Flavoring increased (20 to 40%) the total phenolic contents, whereas oxidative stability was dependent on the flavoring agent (a slight increase for rosemary and a decrease for cinnamon and garlic). Flavoring also had a significant impact on the sensory profiles. Unflavored oils, cinnamon, and garlic flavored oils had a fruity-ripe sensation while rosemary flavored oils were fruity-green oils. Fruit-related sensations, perceived in unflavored oils, disappeared with flavoring. Flavoring decreased the sweetness, enhanced the bitterness, and did not influence the pungency of the oils. According to the EU regulations, flavored oils cannot be commercialized as EVOO. Thus, to guarantee the legal labelling requirement and to meet the expectations of the market-specific consumers for differentiated olive oils, a lab-made electronic nose was applied. The device successfully discriminated unflavored from flavored oils and identified the type of flavoring agent (90 ± 10% of correct classifications for the repeated K-fold cross-validation method). Thus, the electronic nose could be used as a practical non-destructive preliminary classification tool for recognizing olive oils' flavoring practice.

12.
Foods ; 10(3)2021 Feb 25.
Article in English | MEDLINE | ID: mdl-33669026

ABSTRACT

The high proportions of monounsaturated fatty acids (MUFA) represent one of the most important technological and nutritional features of olive oils. The present study details the fatty acid (FA) composition of autochthonous cultivars (Lentisca, Madural, Redondal, Rebolã, Verdeal, and Verdeal Transmontana) produced from centenarian trees during five crop years (2013-2017). Olive cultivar highly influenced the FA composition, namely, oleic acid (70.3% for Madural to 80.7% for Redondal) and palmitic acid (10.4% for Lentisca to 13.5% for Verdeal). Similarly, crop year significantly influenced the individual FA contents. Principal component analysis of FA data enabled the unsupervised classification by cultivar and, within each cultivar, by crop year. Furthermore, the levels of nine individual FAs, together with the polyunsaturated fatty acid contents, selected using the simulated annealing algorithm, allowed for their correct classification, on the basis of linear discriminant analysis, according to the olive cultivar, with an overall sensitivity of 92%, for leave-one-out cross-validation procedure. Globally, the cultivar effect superimposed that of crop year, showing that some cultivars, such as Redondal and Verdeal Transmontana, have consistently high and homogeneous proportions of MUFA, indicating that they are worth exploring in terms of future selection of cultivars that are able to produce olive oils with increased nutritional value and that are less prone to oxidation.

13.
Talanta ; 226: 122122, 2021 May 01.
Article in English | MEDLINE | ID: mdl-33676677

ABSTRACT

An electronic nose, comprising nine metal oxide sensors, has been built aiming to classify olive oils according to the fruity intensity commercial grade (ripely fruity or light, medium and intense greenly fruity), following the European regulated complementary terminology. The lab-made sensor device was capable to differentiate standard aqueous solutions (acetic acid, cis-3-hexenyl, cis-3-hexen-1-ol, hexanal, 1-hexenol and nonanal) that mimicked positive sensations (e.g., fatty, floral, fruit, grass, green and green leaves attributes) and negative attributes (e.g., sour and vinegary defects), as well as to semi-quantitatively classify them according to the concentration ranges (0.05-2.25 mg/kg). For that, unsupervised (principal component analysis) and supervised (linear discriminant analysis: sensitivity of 92% for leave-one-out cross validation) classification multivariate models were established based on nine or six gas sensors, respectively. It was also showed that the built E-nose allowed differentiating/discriminating (sensitivity of 81% for leave-one-out cross validation) extra virgin olive oils according to the perceived intensity of fruitiness as ripely fruity, light, medium or intense greenly fruity. In conclusion, the gas sensor device could be used as a practical preliminary non-destructive tool for guaranteeing the correctness of olive oil fruitiness intensity labelling.

14.
Food Chem ; 337: 127726, 2021 Feb 01.
Article in English | MEDLINE | ID: mdl-32795854

ABSTRACT

Phenolic compounds contribute to the bioactive properties of olive oil. However, olive oils can only support a health claim concerning the protection against oxidative stress depending on the polyphenolic concentration, requiring effective measures during extraction to preserve/enhance their concentrations. The effect of the malaxation temperature (22, 28 and 34 °C) on the phenolic profile was studied for industrially extracted cv. Cobrançosa oils. Higher malaxation temperatures decreased the contents of the majority of the chromatographically detected compounds (P < 0.05, one-way ANOVA), enabling oils' differentiation. This decreasing trend was observed for hydroxytyrosol and tyrosol bound forms, determinant for the health claim, which were also negatively affected by temperature, despite revealing that all the industrially extracted oils tested supported the health claim. The observed constant free to bound forms ratio showed that the temperature range tested had a minor effect on bound-forms hydrolysis, being both free and bound forms equally affected by temperature.


Subject(s)
Health , Olive Oil/chemistry , Phenols/analysis , Temperature , Mechanical Phenomena , Phenols/chemistry
15.
Molecules ; 25(7)2020 Mar 27.
Article in English | MEDLINE | ID: mdl-32230976

ABSTRACT

Replacing synthetic surfactants by natural alternatives when formulating nanoemulsions has gained attention as a sustainable approach. In this context, nanoemulsions based on sweet almond oil and stabilized by saponin from Quillaja bark with glycerol as cosurfactant were prepared by the high-pressure homogenization method. The effects of oil/water (O/W) ratio, total surfactant amount, and saponin/glycerol ratio on their stability were analyzed. The formation and stabilization of the oil-in-water nanoemulsions were analyzed through the evaluation of stability over time, pH, zeta potential, and particle size distribution analysis. Moreover, a design of experiments was performed to assess the most suitable composition based on particle size and stability parameters. The prepared nanoemulsions are, in general, highly stable over time, showing zeta potential values lower than -40 mV, a slight acid behavior due to the character of the components, and particle size (in volume) in the range of 1.1 to 4.3 µm. Response surface methodology revealed that formulations using an O/W ratio of 10/90 and 1.5 wt% surfactant resulted in lower particle sizes and zeta potential, presenting higher stability. The use of glycerol did not positively affect the formulations, which reinforces the suitability of preparing highly stable nanoemulsions based on natural surfactants such as saponins.


Subject(s)
Emulsions/chemistry , Nanostructures/chemistry , Plant Bark/chemistry , Quillaja/chemistry , Saponins/chemistry , Surface-Active Agents/chemistry , Dynamic Light Scattering , Glycerol/chemistry , Hydrogen-Ion Concentration , Particle Size , Plant Oils/chemistry , Water/chemistry
16.
Food Res Int ; 128: 108759, 2020 02.
Article in English | MEDLINE | ID: mdl-31955734

ABSTRACT

Mediterranean olive heritage richness is poorly characterized. Olive oils from minor cultivars of Northeast-Portugal (Lentisca, Madural, Rebolã, Redondal, Verdeal and Verdeal Transmontana) from centenarian trees were chemical and sensory characterized, aiming to identify autochthonous cultivars capable of producing differentiated olive oils. All oils, produced during two campaigns, were classified as extra virgin. Cv. Redondal showed the highest oxidative stability (OS), total phenols, vitamin E and C18:1/C18:2. Contrary, cv. Madural presented the lowest OS and C18:1/C18:2 ratios, supporting the importance of fatty acids on OS, while cv. Verdeal had the lowest total phenols and vitamin E contents. Sensory notes of tomato, apple, dry fruits, fresh herbs, tomato leaves and cabbage were predominant on the oils of most cultivars, whilst some attributes were more specific, such as banana and kiwi (Madural), cherry and apricot (cvs. Lentisca and Madural). The chemical and sensory diversity enabled the statistical discrimination of all cultivars and harvesting years.


Subject(s)
Food Quality , Olea/chemistry , Olive Oil/analysis , Olive Oil/chemistry , Fatty Acids/analysis , Humans , Oxidation-Reduction , Phenols/analysis , Portugal , Vitamin E/analysis
17.
Talanta ; 208: 120364, 2020 Feb 01.
Article in English | MEDLINE | ID: mdl-31816761

ABSTRACT

The identification of more than three perfumes is difficult and no analytical tool can completely replace the human olfactory system for fragrance classification. Indeed, no analytical system can mimic the human fragrance perception, being the recognition of perfume aroma patterns by conventional or sensor-based analytical tools a challenging task. For the perfume sector, the possibility of applying fast, cost-effective and green analytical devices for perfume analysis would represent a huge economic revenue. Since the perfume aroma pattern will depend on the composition of the liquid phase and on the diffusion properties of their volatile components, this work aimed to apply a potentiometric electronic tongue, comprising non-specific cross-sensitive lipid polymeric membranes, combined with chemometric techniques, as a novel perfume classifier. The multisensors device allowed establishing perfumes' unique fingerprints, which were successfully used to discriminate men from women perfumes, to identify the perfume aroma family (Citric-Aromatic, Floral, Floral-Fruity, Floral-Oriental, Floral-Woody, Woody-Oriental and Woody-Spicy) and, assessing the perfume storage time-period (≤ 9 months; 9-24 months; and, ≥ 24 months). The established linear discriminant models were based on single-run potentiometric profiles gathered by sub-sets of sensors selected using the simulated annealing algorithm, which enabled achieving correct classification rates of 93-100% (for leave-one-out cross-validation procedure). The satisfactory performance of the electronic tongue demonstrates the versatility of the proposed approach as a practical perfume preliminary classifier sensor device, which industrial application may be foreseen in a near future, contributing to a green-sustained economic growth of the perfume industry.

18.
Data Brief ; 28: 104908, 2020 Feb.
Article in English | MEDLINE | ID: mdl-31872014

ABSTRACT

The composition of Serra da Estrela PDO cheeses (total fat, total protein, salt and free amino acids) was assessed using NIR spectrophotometry and UPLC-DAD-MS/MS. In total, 24 cheeses were acquired from 6 certified cheesemakers located in 5 different municipalities within the delimited PDO geographical region. Cheeses were produced from raw ewe milk of two autochthonous Portuguese sheep breeds, between November 2017 and March 2018, and were acquired after 45 days of maturation. The data include the mean (and respective standard deviations) levels of moisture (%), total fat (%), total protein (%) and salt (%), obtained by NIR spectrophotometry. As well the mean (and respective standard deviations) of free amino acids contents (mg/100 g of cheese, in wet basis) evaluated using a UPLC-DAD-MS/MS method are shown. The latter data include information regarding 8 essential free amino acids (histidine, leucine-isoleucine, lysine, methionine, phenylalanine, threonine, tryptophan and valine) and 9 non-essential free amino acids (arginine, asparagine, aspartic acid, cysteine, glutamine, glutamic acid, proline, tyrosine and serine). Leucine and isoleucine, being isomers, were quantified together. Leucine-isoleucine, phenylalanine and serine were the most abundant essential free amino acids and cysteine, proline and asparagine were the most abundant non-essential free amino acids. Free amino acids contents depended on the cheese producer as well as on the production time-period.

19.
Food Res Int ; 126: 108729, 2019 12.
Article in English | MEDLINE | ID: mdl-31732033

ABSTRACT

Serra da Estrela cheese is a high-value Portuguese Protected Designation of Origin cheese, produced with raw ewe milk. Thus, information regarding its composition is of utmost relevance for both consumers and certified producers. In this work, the chromatographic profiles of free amino acids in cheeses (45 days of maturation, 6 producers located in 5 municipalities and produced from November 2017 to March 2018) were established by UPLC-DAD-MS/MS. The proposed method allowed detecting 19 free amino acids and cystine with overall limits of detection and quantification lower than 44 µmol/L (1.4 mg/100 g cheese, wet matter) and than 134 µmol/L (4.2 mg/100 g cheese, wet matter), respectively. In all cheeses, 17 free amino acids were quantified including 8 essential amino acids (histidine, leucine-isoleucine, lysine, methionine, phenylalanine, threonine, tryptophan and valine) and 9 non-essential amino acids (arginine, asparagine, aspartic acid, cysteine, glutamic acid, glutamine, proline, serine and tyrosine). The amounts of the free amino acids, essential free amino acids, branched chain free amino acids (leucine, isoleucine and valine) plus the free amino acids ratios (mg/g protein) were further used to identify the producer of Serra da Estrela cheeses. Linear discriminant analysis coupled with the simulated annealing variable selection algorithm was used allowing the correct classification of 96% and 90 ±â€¯8% of the samples, for leave-one-out and repeated K-fold cross-validation procedures, respectively. The satisfactory predictive performance pointed out the possibility of using cheeses' amino acids profiles as origin biomarkers for authenticity control, warranting the correctness identification of the cheese producer/brand, which is quite relevant for ensuring the consumer confidence and satisfaction when purchasing this high-value dairy food.


Subject(s)
Amino Acids/analysis , Cheese/analysis , Cheese/classification , Chromatography, High Pressure Liquid/methods , Tandem Mass Spectrometry/methods , Limit of Detection , Portugal
20.
Talanta ; 197: 363-373, 2019 May 15.
Article in English | MEDLINE | ID: mdl-30771949

ABSTRACT

Olive oil is highly appreciated due to its nutritional and organoleptic characteristics. However, a huge compositional variation is observed between olive oils, requiring the use of diverse analytical techniques for its classification including titration, spectrophotometry and chromatography, as well as sensory analysis. Chemical analysis is usually time-consuming, expensive and require skilled technicians, while the sensorial ones are dependent upon individual subjective evaluations, even if performed by trained panellists. This work evaluated and demonstrated the feasibility of using a potentiometric electronic tongue, comprising non-specific lipid polymeric and cross-sensitive sensor membranes, coupled with chemometric tools based on different sub-sets of sensors (from 11 to 14 sensors), to predict key quality parameters of olive oils based on single-run assays. The multivariate linear models established for 23 centenarian olive trees from different cultivars allowed predicting peroxide value, oxidative stability, total phenols and tocopherols contents, CIELAB scale parameters (L*, a* and b* values), as well as 11 gustatory-retronasal positive attributes (green, sweet, bitter, pungent, tomato and tomato leaves, apple, banana, cabbage, fresh herbs and dry fruits) with satisfactory accuracy (0.90 ±â€¯0.07 ≤ R2 ≤ 0.98 ±â€¯0.02 for the repeated K-fold-CV procedure, which ensured that 25% of the data was used for internal-validation purposes). The electronic tongue device had an accuracy statistically similar to that achieved with standard analytical techniques, pointing out the versatility of the device for the fast and simultaneous chemical and sensory analysis of olive oil.


Subject(s)
Electronic Nose , Olive Oil/analysis , Olive Oil/chemistry , Chemistry, Physical , Potentiometry
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