127 research outputs found

    HPLC with Fluorescence Detection for Determination of Bisphenol A in Canned Vegetables: Optimization, Validation and Application to Samples from Portuguese and Spanish Markets

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    Bisphenol A (BPA) is one of the chemicals used to produce both polycarbonate plastics and epoxy resin coatings. Research has shown that small amounts of BPA can migrate into the foods and beverages enclosed in these types of containers. In this research, an analytical method based on high-performance liquid chromatography with fluorescence detection (HPLC-FLD) was developed and validated for the determination of BPA in canned vegetables. The results were confirmed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) was performed, to identify the coating material of each tin can. Nineteen cans of vegetables were taken as study samples (eleven samples from the Spanish market, and eight samples from the Portuguese market). Excellent linear correlation (r2 = 0.9999) was observed over the range of 0.01 to 0.25 mg/L. Limit of detection (LOD) and limit of quantification (LOQ) values were calculated to be 0.005 mg/kg and 0.01 mg/kg, respectively. Good recoveries, between 72% and 90% were obtained at three different levels of concentration (RSD% = 4.6). BPA was not detected in the samples. The proposed HPLC-FLD was found to be suitable for the determination of BPA in canned vegetablesMF Vaz acknowledges FCT, through IDMEC, under LAETA, project UID/EMS/50022/2019. The work was supported by UIDB/00211/2020 with funding from FCT/MCTES through national funds. Fernanda Vilarinho acknowledges National Institute of Health Dr. Ricardo Jorge through the project “Development of methodologies for the evaluation of polymeric food packaging components and determination of their structural and mechanical properties” (2016 DAN 1289). Antía Lestido Cardama is grateful for her grant “Programa de axudas á etapa predoutoral” da Xunta de Galicia (Conselleriía de Cultura, Educación e Ordenación Universitaria). This research was cofounded by the “Consellería de Cultura, Educación e Ordenación Universitaria, Xunta de Galicia,” reference number GRC 2019/030S

    Determination of Xanthohumol in Hops, Food Supplements and Beers by HPLC

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    Xanthohumol (XN) is the main prenylated chalcone present in hops (Humulus lupulus) with high biological activity, and it is of great importance for human health because of its antioxidant, anti-inflammatory, immunosuppressive and chemopreventive properties. This polyphenol can be included in the diet through foods in which hops are used, such as beer or food supplements. Because of their health benefits and the increasing interest of using hops as a novel nutraceutical, the aim of this work was the identification and quantification of XN in different types of samples using a method based on high resolution liquid chromatography with a diode array detector (HPLC–DAD). The method was validated in terms of linearity, limits of detection (LOD) and quantification (LOQ), repeatability and recovery. Acceptable linearity (r2 0.9999), adequate recovery (>90% in the most of cases) and good sensitivity (LOD 16 µg/L) were obtained. Furthermore, the presence of XN in all samples was confirmed using liquid chromatography coupled to mass spectrometry (LC-MS/MS) operated in negative ESI (electrospray system ionization) mode. The concentrations of XN determined in hop flowers and food supplements were above the LOQ, in a range between 0.106 and 12.7 mg/g. Beer may also represent an important source of dietary prenylflavonoids, with between 0.028 and 0.062 mg/L of XN. The results showed that the methodology proposed was suitable for the determination of XN in the different types of samples studied, and the amounts of XN varied significantly according to the selected productThis research was funded by VIPACFood project (selected by ERA-NET ARIMNet2 call 2016 Coordination of Agricultural Research In the Mediterranean) of the European Union through the 7th Framework Program; and cofunded by the Spanish National Institute for Agricultural and Food Research and Technology (MINECO-INIA), reference APCIN2016-00061-00-00, and by the “Consellería de Cultura, Educación e Ordenación Universitaria, Xunta de Galicia,” reference number GRC 2019/030S

    Study on the chemical behaviour of Bisphenol S during the in vitro gastrointestinal digestion and its bioaccessibility

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    This study evaluated the chemical behaviour of Bisphenol S (BPS) and determined its bioaccessibility after human ingestion using a standardised in vitro gastrointestinal digestion protocol and an analytical method based on high-pressure liquid chromatography coupled with a photodiode array and tandem mass spectrometry. The effects of different factors such as gastric pH, enzymes, and food matrix on the solubility and chemical stability of BPS were studied to evaluate their contribution to its bioaccessibility. The results highlighted that BPS was available at the end of the digestion process in the range of 50–80%, and was susceptible to absorption at the intestinal level. The effect of pH was not significant as a single factor. The presence of enzymes slightly decreased the bioaccessibility of BPS in the intestinal phase with gastric pH increase. Additionally, a soy drink reduced BPS bioaccessibility by up to 5% after oral intake. Finally, a few BPS degradation products were found in non-bioaccessible fractions at different pH valuesThis research was funded the “Consellería de Cultura, Educación e Ordenación Universitaria, Xunta de Galicia”, within the project “Consolidación y estructuración de unidades de investigación competitivas—Grupos de referencia competitiva (GRC)” (Ref. GRC 2019/030). L. Barbosa-Pereira is grateful to the Spanish Ministry of Science, Innovation and Universities for her “Juan de la Cierva – Incorporación” Grant (Agreement No. IJCI-2017-31665). Antía Lestido-Cardama is grateful for her grant “Programa de axudas á etapa predoutoral” da Xunta de Galicia (Consellería de Cultura, Educación e Ordenación UniversitariaS

    Long-term implications of feed energy source in different genetic types of reproductive rabbit females. II.Immunologic status

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    [EN] Genetic selection and nutrition management have played a central role in the development of commercial rabbitry industry over the last few decades, being able to affect productive and immunological traits of the animals. However, the implication of different energy sources in animals from diverse genetic lines achieving such evolutionary success remains still unknown. Therefore, in this work, 203 female rabbits housed and bred in the same conditions were used from their first artificial insemination until their fifth weaning. The animals belonged to three different genetic types diverging greatly on breeding goals (H line, hyper-prolific (n=66); LP line, robust (n=67) and R line, selected for growth rate (n=67), and were assigned to two experimental diets, promoting major differences in energy source (cereal starch or animal fat)). The aims of this work were to: (1) characterize and describe blood leucocyte populations of three lines of rabbit does in different physiological stages during their reproductive period: first artificial insemination, first weaning, second parturition and fifth weaning; and (2) study the possible influence of two different experimental diets on the leucocyte populations in peripheral blood. Flow cytometry analyses were performed on blood samples taken from females at each different sampling stade. Lymphocyte populations at both weanings were characterized by significantly lower counts of total, CD5(+) and CD8(+) lymphocytes (-19.8, -21.7 and -44.6%; P<0.05), and higher counts of monocytes and granulocytes (+49.2 and +26.2%; P<0.05) than in the other stages. Females had higher blood counts of lymphocytes B, CD8(+) and CD25(+) and lower counts of CD4(+) at first than at fifth weaning (+55.6, +85.8, +57.5, -14.5%; P<0.05). G/L ratio was higher at both weanings (P<0.05), and CD4(+)/CD8(+) ratio increased progressively from the 1AI to the 5 W (P<0.001). Regarding the effect of genetic type in blood leucocyte counts, LP animals presented the highest counts for total, B, CD5(+) and CD8(+) lymphocytes (+16.7, +31.8, +24.5 and +38.7; P<0.05), but R rabbits showed the highest counts for monocytes and granulocytes (+25.3 and +27.6; P<0.05). The type of diet given during the reproductive life did not affect the leucocyte population counts. These results indicate that there are detectable variations in the leucocyte profile depending on the reproductive stage of the animal (parturition, weaning or none of them). Moreover, foundation for reproductive longevity criteria allows animals to be more capable of adapting to the challenges of the reproductive cycle from an immunological viewpoint.This study was supported by the Interministerial Commission for Science and Technology (CICYT) of the Spanish Government (AGL2014-53405-C2-1-P; AGL2014-53405-C2-2-P). The authors thank Juan Carlos Moreno for his technical support. Grants for Ana Garcia-Quiros from Universidad CEU-Cardenal Herrera, and Mariola Penades and Alberto Arnau from the Ministerio de Educacion, Cultura y Deporte (AP2010-3907 and BES-2012-052345, respectively) are also gratefully acknowledged.Penadés, M.; Arnau-Bonachera, A.; García-Quirós, A.; Viana, D.; Selva, L.; Corpa, JM.; Pascual Amorós, JJ. (2018). Long-term implications of feed energy source in different genetic types of reproductive rabbit females. II.Immunologic status. 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    Application of chromatographic analysis for detecting components from polymeric can coatings and further determination in beverage samples

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    Major type of internal can coating used for food and beverages is made from epoxy resins, which contain among their components bisphenol A (BPA) or bisphenol A diglycidyl ether (BADGE). These components can be released and contaminate the food or beverage. There is no specific European legislation for coatings, but there is legislation on specific substances setting migration limits. Many investigations have paid attention to BPA due to its classification as endocrine disruptor, however, few studies are available concerning to other bisphenol analogues that have been used in the manufacture of these resins. To evaluate the presence of this family of compounds, ten cans of beverages were taken as study samples. Firstly, the type of coating was verified using an attenuated total reflectance-FTIR spectrometer to check the type of coating presents in most of the samples examined. A screening method was also performed to investigate potential volatiles from polymeric can coatings of beverages using Purge and Trap (P&T) technique coupled to gas chromatography with mass spectrometry detection (GC-MS). Moreover, a selective analytical method based on high performance liquid chromatography with fluorescence detection (HPLC-FLD) for the simultaneous identification and quantification of thirteen compounds including bisphenol analogues (BPA, BPB, BPC, BPE, BPF, BPG) and BADGEs (BADGE, BADGE.H2O, BADGE.2H2O, BADGE.HCl, BADGE.2HCl, BADGE.H2O.HCl, cyclo-di-BADGE) in the polymeric can coatings and in the beverage samples was applied. In addition, a liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) method was optimized for confirmation purposes. The method showed an adequate linearity (R2 >0.9994) and low detection levels down to 5 µg/L. Cyclo-di-BADGE was detected in all extracts of polymeric coatings. The concentrations ranged from 0.004 to 0.60 mg/dm2. No detectable amounts of bisphenol related compounds were found in any of the beverage samples at levels that may pose a risk to human health, suggesting a low intake of bisphenols from beveragesThe study was financially supported by the Ministerio de Ciencia, Innovación y Universidades, by Fondo Europeo de Desarrollo Regional (FEDER), and by Agencia Estatal de Investigación Ref. No. PGC2018-094518-B-I00 “MIGRACOATING” (MINECO/FEDER, UE)S

    Phenolic Profile of Fruit Industry Byproducts Determined by LC–DAD–MS/MS

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    The bioconversion of fruit by-products into new functional and clean label ingredients/additives represents a sustainable approach with great potential for application in the food sectorThis work was financially supported by the VIPACFood project (grant agreement no. 618127) selected by ERA-NET ARIMNet2 call 2016 (Coordination of Agricultural Research in the Mediterranean) of the European Union through the 7th Framework Programme and funding by the Spanish National Institute for Agricultural and Food Research and Technology (INIA) ref. APCIN2016-00061-00-00, by the “Consellería de Cultura, Educación e Ordenación Universitaria, Xunta de Galicia”, Ref. No. GRC 2019/030, and by Foundation for Science and Technology (FCT, Portugal,) ARIMNET2/0003/2016. Cássia H. Barbosa is grateful for her research grant in the frame of the VIPACFood project (ARIMNET2/0003/2016). The work was also supported by UIDB/00211/2020 with funding from FCT/MCTES through national fundsS

    The partial volume effect in the quantification of 1H magnetic resonance spectroscopy in Alzheimer's disease and aging

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    [Abstract] 1H-MRS variability increases due to normal aging and also as a result of atrophy in grey and white matter caused by neurodegeneration. In this work, an automatic process was developed to integrate data from spectra and high-resolution anatomical images to quantify metabolites, taking into account tissue partial volumes within the voxel of interest avoiding additional spectra acquisitions required for partial volume correction. To evaluate this method, we use a cohort of 135 subjects (47 male and 88 female, aged between 57 and 99 years) classified into 4 groups: 38 healthy participants, 20 amnesic mild cognitive impairment patients, 22 multi-domain mild cognitive impairment patients, and 55 Alzheimer's disease patients. Our findings suggest that knowing the voxel composition of white and grey matter and cerebrospinal fluid is necessary to avoid partial volume variations in a single-voxel study and to decrease part of the variability found in metabolites quantification, particularly in those studies involving elder patients and neurodegenerative diseases. The proposed method facilitates the use of 1H-MRS techniques in statistical studies in Alzheimer's disease, because it provides more accurate quantitative measurements, reduces the inter-subject variability, and improves statistical results when performing group comparisons

    Presence of Perfluoroalkyl and Polyfluoroalkyl Substances (PFAS) in Food Contact Materials (FCM) and Its Migration to Food

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    Perfluoroalkyl and polyfluoroalkyl substances (PFAS) are synthetic chemical compounds widely used in different industry fields including food contact materials (FCM), providing resistance to fat and humidity, and non-stick properties. PFAS enter into the food chain directly from the intake of contaminated food or indirectly from the migration of the FCM into the food. This exposure published in different research highlights a public health concern. Therefore, it is necessary to perform analysis of the content of different FCM and evaluate the migration from the FCM under normal conditions of use and storage. This bibliographical review proves that different perfluoroalkyl and polyfluoroalkyl compounds are detected in fast food packaging, microwave popcorn bags, and frying pans, among others. Furthermore, it shows the conditions or factors that favor the migration of the PFAS from the FCM into the foodThis research was funded by the Consellería de Cultura, Eduación e Ordenación Universitaria, Xunta de Galicia, within the project “Consolidación y estructuración de unidades de investigación competitivas—Grupos de referencia competitiva (GRC)” Ref. No. GRC ED431C 2019/30. P.V.L. acknowledges to “Ministerio de Ciencia, Innovación y Universidades” for her Predoctoral fellowship (ref. PRE2019-088195); A.L.C. is grateful for her grant “Programa de axudas á etapa predoutoral” da Xunta de Galicia (Consellería de Cultura, Educación e Ordenación Universitaria). L.B.P. is grateful to the Spanish Ministry of Science, Innovation and Universities for her “Juan de la Cierva—Incorporación” Grant (Agreement No. IJCI- 2017-31665)S

    GC-MS screening for the identification of potential migrants present in polymeric coatings of food cans

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    The coatings used in cans can release complex chemical mixtures into foodstuffs. Therefore, it is important to develop analytical methods for the identification of these potential migrant compounds in packaged food to guarantee the compliance with European food packaging legislation and ensure consumer safety. In the present work, the type of coating in a total of twelve cans collected in Santiago de Compostela (Spain) were evaluated using an ATR (attenuated total reflectance)-FTIR spectrometer. These samples were analysed after extraction with acetonitrile in order to identify potential migrants through a screening method by gas chromatography coupled to mass spectrometry (GC-MS). A total of forty-seven volatile and semi-volatile compounds were identified in these samples, including plasticizers, photoinitiators, antioxidants, lubricants, etc. Then, in a second step, a targeted analysis was carried out for the simultaneous determination of 13 compounds, including bisphenols (BPA, BPB, BPC, BPE, BPF, BPG) and BADGEs (BADGE, BADGE.H2O, BADGE.2H2O, BADGE.HCl, BADGE.2HCl, BADGE.H2O.HCl, cyclo-di-BADGE) by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) with atmospheric pressure chemical ionisation (APCI) source. Among all the bisphenols analysed, only the bisphenol A was detected in four samples; while cyclo-di-BADGE was the predominant compound detected in all the samples analysed.This research was funded by the Ministerio de Ciencia, Innovación y Universidades, by Fondo Europeo de Desarrollo Regional (FEDER), and by Agencia Estatal de Investigación Ref.No. PGC2018-094518-B-I00 “MIGRACOATING” (MINECO/FEDER, UE)S
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