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ABSTRACT: Nowadays, new emerging products claiming antioxidant properties are becoming more frequent. However, information about this topic in their labels is usually scarce. In this paper, we analyzed total phenolics, total flavonoids and ascorbic acid contents, as well as DPPH scavenging activity of several commercial samples, namely green tea and other herbal infusions, dietary supplements, and fruit juices, available in the Portuguese market. In general, beverages containing green tea and hibiscus showed higher phenolics contents (including flavonoids) and antioxidant activity than those without these ingredients. A borututu infusion presented the lowest concentrations of bioactive compounds and scavenging activity, due to the low recommended amount of plant to prepare the beverage. Some juices without antioxidant claims in the label presented similar values to those with it.
Lebensmittel-Wissenschaft und-Technologie 12/2012; 49(2):324–328. · 2.55 Impact Factor
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ABSTRACT: In Portugal, commercial milk is obtained almost entirely from cows of the Holstein breed. However, other breeds may also show dairy aptitude, and produce milk of good quality. The aim of this study was to investigate the effect of the breed factor in the vitamin contents of milks from Holstein and the autochthonous Portuguese breed Minhota, as well as possible variations due to season. Milk samples were collected from 15 cows of each breed. Milk from Minhota cows showed higher contents of retinol, retinyl palmitate, α-tocopherol, and β-carotene. No differences were verified between breeds regarding vitamin D(3) content, but Holstein cows presented higher amounts of provitamin D(3). Seasonal variations were not observed for milk samples from Holsteins, and only a very small variation was observed for milk samples from Minhota cows, mainly in retinol, α-tocopherol, and provitamin D(3) levels. This study revealed that breed has a pronounced effect on milk fat-soluble vitamins, which is an important observation regarding future genetic selection plans. Also, the increased vitamin amounts found in milk from Minhota cows can be regarded as an important nutritional parameter that can potentiate the economical value of this breed.
Journal of Dairy Science 08/2012; 95(10):5476-84. · 2.56 Impact Factor
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ABSTRACT: Solid-phase microextraction (SPME) is a simple, fast, economic and solvent-free sample preparation technique that has, among
other applications, been used to measure the volatile flavor profiles of foods and beverages.
The objective of our study was to optimize the application of SPME-GC for analysis of volatile compounds in ewe cheeses. The
volatile compounds in cheese were extracted by immersing the fiber coating in the sample headspace. The effects of fiber coating,
exposure time, and sample and headspace volumens were investigated. The optimized methodology was suitable for studying the
profiles of volatile compounds in ewe cheese during ripening. The advantages and limitations of SPME in the analysis of volatile
compounds in cheese are discussed.
Chromatographia 04/2012; 53:S390-S393. · 1.20 Impact Factor
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Food Chemistry 01/2012; · 3.65 Impact Factor
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ABSTRACT: To counteract and prevent the deleterious effect of free radicals the living organisms have developed complex endogenous and exogenous antioxidant systems. Several analytical methodologies have been proposed in order to quantify antioxidants in food, beverages and biological fluids. This paper revises the electroanalytical approaches developed for the assessment of the total or individual antioxidant capacity. Four electrochemical sensing approaches have been identified, based on the direct electrochemical detection of antioxidant at bare or chemically modified electrodes, and using enzymatic and DNA-based biosensors.
Biosensors & bioelectronics 09/2011; 30(1):1-12. · 5.43 Impact Factor
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ABSTRACT: The antioxidant profiles of 39 water samples (29 flavored waters based on 10 natural waters) and 6 flavors used in their formulation (furnished by producers) were determined. Total phenol and flavonoid contents, reducing power, and DPPH radical scavenging activity were the optical techniques implemented and included in the referred profile. Flavor extracts were analyzed by HS-SPME/GC-MS to obtain the qualitative and quantitative profiles of the volatile fraction of essential oils. Results pointed out a higher reducing power (0.14-11.8 mg of gallic acid/L) and radical scavenging activity (0.29-211.5 mg Trolox/L) of flavored waters compared with the corresponding natural ones, an interesting fact concerning human health. Bioactive compounds, such as polyphenols, were present in all samples (0.5-359 mg of gallic acid/L), whereas flavonoids were not present either in flavored waters or in flavors. The major components of flavor extracts were monoterpenes, such as citral, α-limonene, carveol, and α-terpineol.
Journal of Agricultural and Food Chemistry 04/2011; 59(9):5062-72. · 2.82 Impact Factor
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ABSTRACT: In this paper, a biosensor based on a glassy carbon electrode (GCE) was used for the evaluation of the total antioxidant capacity (TAC) of flavours and flavoured waters. This biosensor was constructed by immobilising purine bases, guanine and adenine, on a GCE. Square wave voltammetry (SWV) was selected for the development of this methodology. Damage caused by the reactive oxygen species (ROS), superoxide radical (O(2)·(-)), generated by the xanthine/xanthine oxidase (XOD) system on the DNA-biosensor was evaluated. DNA-biosensor encountered with oxidative lesion when it was in contact with the O(2)·(-). There was less oxidative damage when reactive antioxidants were added. The antioxidants used in this work were ascorbic acid, gallic acid, caffeic acid, coumaric acid and resveratrol. These antioxidants are capable of scavenging the superoxide radical and therefore protect the purine bases immobilized on the GCE surface. The results demonstrated that the DNA-based biosensor is suitable for the rapid assess of TAC in beverages.
Biosensors & bioelectronics 02/2011; · 5.43 Impact Factor
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ABSTRACT: Three commonly consumed and commercially valuable fish species (sardine, chub and horse mackerel) were collected from the Northeast and Eastern Central Atlantic Ocean in Portuguese waters during one year. Mercury, cadmium, lead and arsenic amounts were determined in muscles using graphite furnace and cold vapour atomic absorption spectrometry. Maximum mean levels of mercury (0.1715 ± 0.0857 mg/kg, ww) and arsenic (1.139 ± 0.350 mg/kg, ww) were detected in horse mackerel. The higher mean amounts of cadmium (0.0084 ± 0.0036 mg/kg, ww) and lead (0.0379 ± 0.0303 mg/kg, ww) were determined in chub mackerel and in sardine, respectively. Intra- and inter-specific variability of metals bioaccumulation was statistically assessed and species and length revealed to be the major influencing biometric factors, in particular for mercury and arsenic. Muscles present metal concentrations below the tolerable limits considered by European Commission Regulation and Food and Agriculture Organization of the United Nations/World Health Organization (FAO/WHO). However, estimation of non-carcinogenic and carcinogenic health risks by the target hazard quotient and target carcinogenic risk, established by the US Environmental Protection Agency, suggests that these species must be eaten in moderation due to possible hazard and carcinogenic risks derived from arsenic (in all analyzed species) and mercury ingestion (in horse and chub mackerel species).
Food and chemical toxicology: an international journal published for the British Industrial Biological Research Association 12/2010; 49(4):923-32. · 2.99 Impact Factor
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ABSTRACT: Reactive oxygen species (ROS) are produced as a consequence of normal aerobic metabolism and are able to induce DNA oxidative damage. At the cellular level, the evaluation of the protective effect of antioxidants can be achieved by examining the integrity of the DNA nucleobases using electrochemical techniques. Herein, the use of an adenine-rich oligonucleotide (dA(21)) adsorbed on carbon paste electrodes for the assessment of the antioxidant capacity is proposed. The method was based on the partial damage of a DNA layer adsorbed on the electrode surface by OH radicals generated by Fenton reaction and the subsequent electrochemical oxidation of the intact adenine bases to generate an oxidation product that was able to catalyze the oxidation of NADH. The presence of antioxidant compounds scavenged hydroxyl radicals leaving more adenines unoxidized, and thus, increasing the electrocatalytic current of NADH measured by differential pulse voltammetry (DPV). Using ascorbic acid (AA) as a model antioxidant species, the detection of as low as 50 nM of AA in aqueous solution was possible. The protection efficiency was evaluated for several antioxidant compounds. The biosensor was applied to the determination of the total antioxidant capacity (TAC) in beverages.
Biosensors & bioelectronics 10/2010; 26(5):2396-401. · 5.43 Impact Factor
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ABSTRACT: The antioxidant properties of almond green husks (Cvs. Duro Italiano, Ferraduel, Ferranhês, Ferrastar and Orelha de Mula), chestnut skins and chestnut leaves (Cvs. Aveleira, Boa Ventura, Judia and Longal) were evaluated through several chemical and biochemical assays in order to provide a novel strategy to stimulate the application of waste products as new suppliers of useful bioactive compounds, namely antioxidants. All the assayed by-products revealed good antioxidant properties, with very low EC(50) values (lower than 380 μg/mL), particularly for lipid peroxidation inhibition (lower than 140 μg/mL). The total phenols and flavonoids contents were also determined. The correlation between these bioactive compounds and DPPH (2,2-diphenyl-1-picrylhydrazyl) radical scavenging activity, reducing power, inhibition of β-carotene bleaching and inhibition of lipid peroxidation in pig brain tissue through formation of thiobarbituric acid reactive substances, was also obtained. Although, all the assayed by-products proved to have a high potential of application in new antioxidants formulations, chestnut skins and leaves demonstrated better results.
Food Science and Technology International 06/2010; 16(3):209-16. · 0.68 Impact Factor
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ABSTRACT: Dust is the repository of various compounds including flame retardants. In this study an analytical method based on PLE extraction and gas chromatography-mass spectrometry was selected for the analysis of 16 PBDEs congeners in house and car dust samples collected in Portugal. The analytical performance of the method was validated using standard reference material (SRM); values from 90% to 109% and from 2% to 11% were obtained for recovery and precision, respectively. The PBDE congeners distribution in whole and sieved fractions of the dust samples, as well as influence of the source on the levels of these contaminants, were obtained. The wide range of PBDEs contents found in the dust samples indicates heterogeneous levels of contamination in these matrices. The clearest feature of the results obtained was that Deca-BDE was the main PBDE in both house and car dust samples. The total PBDEs measured in house dust (ranging from 34 to 1928 ng g(-1)) was lower than those found in car dust (ranging from 193 to 22955 ng g(-1)). However, house dust provides a major contribution to human exposure due to the time spent there, much higher than in cars.
Chemosphere 03/2010; 78(10):1263-71. · 3.21 Impact Factor
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S Duarte,
J Bento,
A Pena,
C M Lino,
C Delerue-Matos,
T Oliva-Teles,
S Morais,
M Correia, M B P P Oliveira,
M R Alves,
J A Pereira
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ABSTRACT: Ochratoxin A (OTA) is a mycotoxin produced by a variety of fungi, such as Penicillium verrucosum and Aspergillium spp., which has been found to have a wide number of potentially deadly toxic effects, and can enter the human organism through a variety of means. It then finds its way into the bloodstream and, after a lengthy process, is eventually excreted through the urine. It can thus be detected in its original form not only in blood samples but also in this biological medium. As such, and in an attempt to evaluate the exposure of the Portuguese population to this mycotoxin, morning urine samples were collected during the Winter of 2007, from each of five geographically distinct Portuguese locations--Bragança, Porto, Coimbra, Alentejo, and Algarve--and subjected to extraction by immunoaffinity columns and to OTA quantification through liquid chromatography coupled with fluorescence detection. Prevalent incidence was higher than 95% with Coimbra being the exception (incidence of 73.3%). In nearly all locations, the OTA content of most samples was found to be above the limit of quantification (LOQ) of 0.008 ng/ml. Indeed, excluding Coimbra, with an OTA content level of 0.014 ng/ml, all regions featured content values over 0.021 ng/ml.
Science of The Total Environment 12/2009; 408(5):1195-8. · 3.29 Impact Factor
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ABSTRACT: Concentrations of eleven trace elements (Al, As, Cd, Cr, Co, Hg, Mn, Ni, Pb, Se, and Si) were measured in 39 (natural and flavoured) water samples. Determinations were performed using graphite furnace electrothermetry for almost all elements (Al, As, Cd, Cr, Co, Mn, Ni, Pb, and Si). For Se determination hydride generation was used, and cold vapour generation for Hg. These techniques were coupled to atomic absorption spectrophotometry. The trace element content of still or sparkling natural waters changed from brand to brand. Significant differences between natural still and natural sparkling waters (p < 0.001) were only apparent for Mn. The Mann–Whitney U-test was used to search for significant differences between flavoured and natural waters. The concentration of each element was compared with the presence of flavours, preservatives, acidifying agents, fruit juice and/or sweeteners, according to the labelled composition. It was shown that flavoured waters generally increase the trace element content. The addition of preservatives and acidifying regulators had a significant influence on Mn, Co, As and Si contents (p < 0.05). Fruit juice can also be correlated to the increase of Co and As. Sweeteners did not provide any significant difference in Mn, Co, Se and Si content.
Food Additives and Contaminants Part B 11/2009; 2(2):121-130. · 0.89 Impact Factor
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ABSTRACT: A method for the rapid trace analysis of 24 residual pesticides in apple juice by multidimensional gas chromatography-mass spectrometry (MD-GC/MS) using dispersive liquid-liquid microextraction (DLLME) was developed and optimized. Several parameters of the extraction procedure such as type and volume of extraction solvent, type and volume of dispersive solvent and salt addition were evaluated to achieve the highest yield and to attain the lowest detection limits. The DLLME procedure optimized consists in the formation of a cloudy solution promoted by the fast addition to the sample (5 ml) of a mixture of carbon tetrachloride (extraction solvent, 100 microl) and acetone (dispersive solvent, 400 microl). The tiny droplets formed and dispersed among the aqueous sample solution are further joined and sedimented (85 microl) in the bottom of the conical test tube by centrifugation. Once extracted, all the 24 pesticides were directly injected and separated by a dual GC column system, comprising a short wide-bore DB-5 capillary column with low film thickness connected by a Deans switch system to a second chromatographic narrower column, with identical stationary phase. The instrumental setting used, in combination with carefully optimized operational fast GC and MS parameters, markedly decreased the retention times of the targeted analytes. The total chromatographic run was 8 min. Mean recoveries for apple juice spiked at three concentrations ranged from 60% to 105% and the intra-repeatability ranged from 1% to 21%. The limits of detection of the 24 pesticides ranged from 0.06 to 2.20 microg/L. In 2 of a total of 28 analysed samples were found residues of captan, although at levels below the maximum limit legal established.
Journal of chromatography. A 10/2009; 1216(51):8835-44. · 4.19 Impact Factor
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ABSTRACT: A fast method using low-pressure gas chromatography coupled to mass spectrometry (LP-GC/MS) was implemented and optimized to yield a complete separation of 27 representative pesticides in grapes, musts and wines. Extraction was performed with acetonitrile, applying quick, easy, cheap, effective, rugged and safe (QuEChERS) methodology. Several LP-GC/MS conditions such as column temperature, injection conditions, flow rate, MS conditions and matrix effects were evaluated to achieve the fastest separation with the highest sensitivity in MS detection (selected ion monitoring mode). After optimization, all 27 pesticides were extracted, chromatographically separated and detected in less than 20 min. Acceptable recoveries for nearly all pesticides at three different spiking levels (from 0.04 to 2.5 microg/g) were achieved with good repeatability (from 3 to 21%). Limits of quantification (from 0.02 to 5 microg/g) were lower than the maximum limit of residues, when established for pesticides.
Journal of Chromatography 12/2008; 1216(1):119-26. · 4.53 Impact Factor
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ABSTRACT: A derivatization method for the analysis of 12 heterocyclic aromatic amines (HAs) in food, by gas chromatography-electron impact mass spectrometry, was developed. The amines are derivatized in a one-step reaction with N-methyl-N-(tert.-butyldimethylsilyl)trifluoroacetamide. The derivatives are characterized by easy-to-interpret mass spectra due to the prominent ion [M-57]+ by loss of a tert.-butyldimethylsilyl group, allowing quantification in the selected-ion monitoring mode at the picogram level. The effect of temperature, time, and reagents on the formation of the derivatives was monitored in detail. Quality parameters were evaluated in the optimum working conditions. This derivatization method is not applicable to the pyridoimidazoles Glu-P-1 and Glu-P-2 and to the beta-carboline harman due to incompletely derivatization. The instability of the imidazolquinoline and imidazoquinoxaline derivatives, requiring their injection on the same working day, is a further drawback. This simple, rapid and accurate derivatization procedure is suitable for routine analysis, as illustrated by the analysis of some common foods.
Journal of Chromatography 07/2004; 1040(1):105-14. · 4.53 Impact Factor
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ABSTRACT: Twenty-four coffee samples of different botanical and geographical origins were analyzed for their FA composition, including
trans isomers. The analysis used high-resolution GC/FID/CP Sil 88 capillary column to separate FAME obtained by esterification
with BF3/methanol. The purpose of this work was to verify whether this parameter could be applied in the discrimination of arabica and robusta coffees, either in green or in roasted stage. Statistical approaches were applied to check the efficiecies of some univariate
and multivariate procedures, and the results permitted the conclusion that the FA profile can be used as a coffee variety
marker and may inform on the historical background, mainly in terms of heat-processing conditions.
Journal of Oil & Fat Industries 05/2003; 80(6):511-517. · 1.77 Impact Factor
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ABSTRACT: A GC-MS method is described for quantification of 4-(5-)methylimidazole (4MI) in coffee. Although tested, GC-flame ionization detection proved inadequate for this purpose due to the complexity of the coffee matrix. The developed method was based on ion-pair extraction with bis-2-ethylhexylphosphate and derivatization with isobutylchloroformate. Quantification was carried out by the standard addition method using 2-ethylimidazole as internal standard. Reproducibility data from the complete procedure are presented. Mean recoveries were higher than 98%. The method was applied to green and roasted coffee samples from the two most important varieties, arabica and robusta, and to commercial "torrefacto" coffee blends. 4MI was not detected in the green coffee samples analysed and ranged from 0.307 to 1.241 mg/kg in roasted samples.
Journal of Chromatography 12/2002; 976(1-2):285-91. · 4.53 Impact Factor
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ABSTRACT: Olives (Olea europaea cv. Cobrançosa, Madural, and Verdeal Transmontana) used for oil production were stored, in plastic containers, at 5 +/- 2 degrees C (70% relative humidity) for three different periods before oil extraction: 0, 7, and 14 days (T(0), T(7), and T(14), respectively). In the crop year 1997/1998 this procedure was done only for cv. Cobrançosa and in 1998/1999 for the three cultivars. After storage, the oils were extracted from the fruits, and the acidity, peroxide value, coefficients of specific extinction at 232 and 270 nm, stability, color, p-anisidine value, fatty acids, and tocopherols compositions were determined. The results confirm that storage of fruits produces losses in the olive oil quality. Acidity and stability to oxidation indicate a progressive deterioration of oil quality as fruit is stored. The storage time affects the total tocopherols contents, namely, alpha-tocopherol, which clearly decreased during fruit storage. The oil quality of the Verdeal Transmontana cultivar deteriorated more rapidly than that of Cobrançosa and Madural cultivars. This study also shows that cv. Cobrançosa, the main cultivar in the region, is a good choice in terms of final olive oil quality.
Journal of Agricultural and Food Chemistry 11/2002; 50(22):6335-40. · 2.82 Impact Factor
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CyTA - Journal of Food 01/1998; 2(1):24-32. · 0.63 Impact Factor
