¿Son fiables los productos que encontramos en los supermercados?

Duración (en horas): De 21 a 30 horas. Destinatario: EstudianteEn este recurso didáctico se presenta la metodología en base a proyectos utilizada en el proceso de enseñanza-aprendizaje de la asignatura optativa "Cromatografía y Técnicas Afines" que se imparte en el segundo ciclo de la Licenciatura de Química. El proyecto, que lleva como título "¿Son fiables los productos que encontramos en los supermercados?", permite al alumno aprender los distintos métodos analíticos para el analisis de contaminantes en los productos alimenticios, pero a su vez comprender todos aquellos aspectos teórico-prácticos de la cromatografía y las técnicas afines. En este sentido, cada vez es mayor la información y las noticias que nos llegan sobre la contaminación de los productos alimenticios. Podemos encontrar un amplio número de ejemplos en la última década como la contaminación de pollos con dioxinas en Bélgica y Alemania, la contaminación de leche para niños con melanina en China, etc. Estos casos suscitan una gran preocupación en la sociedad sobre la calidad de los productos alimenticios así como el interés de plantear reglamentación sobre los alimentos que garanticen el control de la calidad de los mismos. Este proyecto, por lo tanto, irá encaminado al desarrollo de determinados métodos analíticos que pueden ser aplicados en el departamento de la unidad de análisis de alimentos que garanticen su calidad y el bienestar del consumidor, como son, por ejemplo: a) Objetivos marcados por el responsable del laboratorio de cromatografía de gases: análisis de bifenilos policlorados en peces, la elección de un inyector adecuado para el análisis de furano en café, y el análisis de melanina en leche en polvo. b) Con lo que respecta al laboratorio de Cromatografía de Líquidos los objetivos marcados son: determinación de clenbuterol, salbutamol y cimateol en carne y la detección de determinados problemas analíticos detectados en distintos métodos analíticos y su resolución

Magnetic properties of cherts from the basque-cantabrian basin and surrounding regions: Archeological implications

We present the first rock magnetic study of archeologically-relevant chert samples from the Basque-Cantabrian basin (BCB) and surrounding regions, which was conducted in order to test the usefulness of non-destructive magnetic properties for assessing chert quality, distinguishing source areas, and identifying heated samples in the archeological record. Our results indicate that the studied BCB cherts are diamagnetic and have very low amounts of magnetic minerals. The only exception is the chert of Artxilondo, which has a median positive magnetic susceptibility associated with larger concentrations of magnetic minerals. But even in this case, the magnetic susceptibility is within the lower range of other archeologically-relevant cherts elsewhere, which indicates that the studied BCB cherts can be considered as flint. The similar median values for all magnetic properties, along with their associated large interquartile ranges, indicates that rock magnetic methods are of limited use for sourcing different types of flint except in some specific contexts involving the Artxilondo flint. With regards to the identification of chert heating in the archeological record, our results indicate only a minor magnetic enhancement of BCB natural flint samples upon heating, which we attribute to the low amount of non-silica impurities. In any case, the diamagnetic behavior of most BCB natural flints, along with the local use only of the Artxilondo type, suggests that any flint tool within the core of the BCB with positive magnetic susceptibility values is likely to have been subjected to heating for improving its knapping properties. Further studies are necessary to better identify the type, origin and grain size of magnetic minerals in BCB natural flints, and to apply non-destructive magnetic properties to flint tools in order to identify the use of heat treatment in the BCB archeological record. © 2016 Larrasoaña, Beamud, Olivares, Murelaga, Tarriño, Baceta and Etxebarria.This study was funded by project GUI15/34 of the Universidad del País Vasco.Peer reviewe

Chitosan-Coated Alginate Microcapsules of a Full-Spectrum Cannabis Extract: Characterization, Long-Term Stability and In Vitro Bioaccessibility

Cannabinoids present in Cannabis sativa are increasingly used in medicine due to their therapeutic potential. Moreover, the synergistic interaction between different cannabinoids and other plant constituents has led to the development of full-spectrum formulations for therapeutic treatments. In this work, the microencapsulation of a full-spectrum extract via vibration microencapsulation nozzle technique using chitosan-coated alginate is proposed to obtain an edible pharmaceutical-grade product. The suitability of microcapsules was assessed by their physicochemical characterization, long-term stability in three different storage conditions and in vitro gastrointestinal release. The synthetized microcapsules contained mainly ∆9-tetrahydrocannabinol (THC)-type and cannabinol (CBN)-type cannabinoids and had a mean size of 460 ± 260 µm and a mean sphericity of 0.5 ± 0.3. The stability assays revealed that capsules should be stored only at 4 °C in darkness to maintain their cannabinoid profile. In addition, based on the in vitro experiments, a fast intestinal release of cannabinoids ensures a medium–high bioaccessibility (57–77%) of therapeutically relevant compounds. The full characterization of microcapsules indicates that they could be used for the design of further full-spectrum cannabis oral formulations.This research was funded by the Basque Government through the financial support as consolidated group of the Basque Research System (IT1213-19 and IT1446-22)

From target analysis to suspect and non-target screening of endocrine-disrupting compounds in human urine

[EN] In the present work, a target analysis method for simultaneously determining 24 diverse endocrine-disrupting compounds (EDCs) in urine (benzophenones, bisphenols, parabens, phthalates and antibacterials) was developed. The target analysis approach (including enzymatic hydrolysis, clean-up by solid-phase extraction and analysis by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS)) was optimized, validated and applied to volunteers' samples, in which 67% of the target EDCs were quantified. For instance, benzophenone-3 (0.2-13 ng g(-1)), bisphenol A (7.7-13.7 ng g(-1)), methyl 3,5-dihydroxybenzoate (8-254 ng g(-1)), mono butyl phthalate (2-17 ng g(-1)) and triclosan (0.3-9 ng g(-1)) were found at the highest concentrations, but the presence of other analogues was detected as well. The developed target method was further extended to suspect and non-target screening (SNTS) by means of LC coupled to high-resolution MS/MS. First, well-defined workflows for SNTS were validated by applying the previously developed method to an extended list of compounds (83), and then, to the same real urine samples. From a list of approximately 4000 suspects, 33 were annotated at levels from 1 to 3, with food additives/ingredients and personal care products being the most abundant ones. In the non-target approach, the search was limited to molecules containing S, Cl and/or Br atoms, annotating 4 pharmaceuticals. The results from this study showed that the combination of the lower limits of detection of MS/MS and the identification power of high-resolution MS/MS is still compulsory for a more accurate definition of human exposome in urine samples.Open Access funding provided thanks to the CRUE-CSIC agreement with Springer Nature. This work has been financially supported by the Ministry of Science and Innovation of the Spanish Government through project PID2020-117686RB-C31, and by the Education Department of the Basque Government as a consolidated group of the Basque Research System (IT1213-19)

Dilute-and-shoot coupled to mixed mode liquid chromatography-tandem mass spectrometry for the analysis of persistent and mobile organic compounds in human urine

In this work, a comprehensive method for the simultaneous determination of 33 diverse persistent and mobile organic compounds (PMOCs) in human urine was developed by dilute-and-shoot (DS) followed by mixed-mode liquid chromatography coupled with tandem mass spectrometry (MMLC-MS/MS). In the sample preparation step, DS was chosen since it allowed the quantification of all targets in comparison to lyophilization. For the chromatographic separation, Acclaim Trinity P1 and P2 trimodal columns provided greater capacity for retaining PMOCs than reverse phase and hydrophilic interaction liquid chromatography. Therefore, DS was validated at 5 and 50 ng/mL in urine with both mixed mode columns at pH = 3 and 7. Regarding figures of merit, linear calibration curves (r2 > 0.999) built between instrumental quantification limits (mostly below 5 ng/mL) and 500 ng/mL were achieved. Despite only 60% of the targets were recovered at 5 ng/mL because of the dilution, all PMOCs were quantified at 50 ng/mL. Using surrogate correction, apparent recoveries in the 70–130% range were obtained for 91% of the targets. To analyse human urine samples, the Acclaim Trinity P1 column at pH = 3 and 7 was selected as a consensus between analytical coverage (i.e. 94% of the targets) and chromatographic runs. In a pooled urine sample, industrial chemicals (acrylamide and bisphenol S), biocides and their metabolites (2-methyl-4-isothiazolin-3-one, dimethyl phosphate, 6-chloropyridine-3-carboxylic acid, and ammonium glufosinate) and an artificial sweetener (aspartame) were determined at ng/mL levels. The outcomes of this work showed that humans are also exposed to PMOCs due to their persistence and mobility, and therefore, further human risk assessment is needed.Authors gratefully acknowledge financial support from the State Research Agency of the Ministry of Science and Innovation (Government of Spain) through project PID2020–117686RB-C31 and the Basque Government as a consolidated group of the Basque Research System (IT-1446–22). M. Musatadi also acknowledges the Basque Government for his predoctoral grant

Metabolomics to study the sublethal effects of diazepam and irbesartan on glass eels (Anguilla anguilla)

Since glass eels are continuously exposed to contamination throughout their migratory journey in estuaries, to a certain extent the fall in the population of this endangered species might be attributed to this exposure, which is especially acute in estuaries under high urban pressure. In this work, metabolomics was used to address the main objective of this study, to evaluate the effects of two pharmaceuticals previously identified as potential concerning chemicals for fish (diazepam and irbesartan) on glass eels. An exposure experiment to diazepam, irbesartan and their mixture was carried out over 7 days followed by 7 days of depuration phase. After exposure, glass eels were individually sacrificed using a lethal bath of anesthesia, and then an unbiased sample extraction method was used to extract separately the polar metabolome and the lipidome. The polar metabolome was submitted to targeted and non-targeted analysis, whereas for the lipidome only the non-targeted analysis was carried out. A combined strategy using partial least squares discriminant analysis and univariate and multivariate statistical analysis (ANOVA, ASCA, t-test, and fold-change analysis) was used to identify the metabolites altered in the exposed groups with respect to the control group. The results of the polar metabolome analysis revealed that glass eels exposed to the diazepam-irbesartan mixture were the most impacted ones, with altered levels for 11 metabolites, some of them belonging to the energetic metabolism, which was confirmed to be sensitive to these contaminants. Additionally, the dysregulation of the levels of twelve lipids, most of them with energetic and structural functions, was also found after exposure to the mixture, which might be related to oxidative stress, inflammation, or alteration of the energetic metabolism.Authors acknowledge financial support from the Agencia Estatal de Investigación (AEI) of Spain and the European Regional Development Fund through CTM2017–84763-C3–1-R and CTM2020–117686RB-C31 projects and the Basque Government through the financial support as a consolidated group of the Basque Research System (IT1446–22). Naroa Lopez-Herguedas is grateful to the Spanish Ministry of Economy, Industry and Competitivity for her predoctoral scholarship FPI 2018. Iker Alvarez-Mora is grateful to the University of the Basque Country and the Université de Pau et des Pays de L' Adour for his cotutelle predoctoral scholarship

Konposatu kannabinoideen analisia matrize biologikoetan: odola, plasma, gernua, listua eta ilea

Cannabis Sativa edo marihuana, Europar Batasunean gehien kontsumitzen den legez kanpoko droga da. ..9-THC-a, Cannabis Sativaren osagai nagusiaren efektu psikoaktiboak istripu edota ondorio latzen eragile izan daitekeenez, beharrezkoa gertatzen da Cannabis Sativa noiz eta zenbat kontsumitu den jakitea edozein istripu ikerketa batean argibideak izateko. Egun, uneko analisi azkarrak jasotzen ahalbideratzen duten detektagailuak erabili daitezkeen arren, beharrezkoak gertatzen dira matrize biologikoetan ..9-THC-aren analisi zehatz eta sentikorrak ahalbidetzen dituzten analisi metodoen garapen eta erabilera. Lan honetan beraz, Cannabis Sativaren osagai psikoaktiboen eta beraien metabolitoen analisia egiteko hainbat analisi metodo laburbiltzen dira lau lagin biologikotan: odolean, gernuan, listuan eta ilean hain zuzen ere

Konposatu kannabinoideen analisia matrize biologikoetan: odola, plasma, gernua, listua eta ilea

Cannabis Sativa edo marihuana, Europar Batasunean gehien kontsumitzen den legez kanpoko droga da. ..9-THC-a, Cannabis Sativaren osagai nagusiaren efektu psikoaktiboak istripu edota ondorio latzen eragile izan daitekeenez, beharrezkoa gertatzen da Cannabis Sativa noiz eta zenbat kontsumitu den jakitea edozein istripu ikerketa batean argibideak izateko. Egun, uneko analisi azkarrak jasotzen ahalbideratzen duten detektagailuak erabili daitezkeen arren, beharrezkoak gertatzen dira matrize biologikoetan ..9-THC-aren analisi zehatz eta sentikorrak ahalbidetzen dituzten analisi metodoen garapen eta erabilera. Lan honetan beraz, Cannabis Sativaren osagai psikoaktiboen eta beraien metabolitoen analisia egiteko hainbat analisi metodo laburbiltzen dira lau lagin biologikotan: odolean, gernuan, listuan eta ilean hain zuzen ere

Dimentsio biko gas-kromatografia dimentsio bakarreko gas-kromatografiaren beharrak asetzen

Gas-kromatografia teknika oso hedatua dago analisi kimikoan, osagai kimikoak bereiztu, identifikatu, detektatu eta kuantifikatu nahi direnean. Analisi teknika honen ibilbidea ezaguna eta garatua bada ere, konplexutasun handiko laginen analisia egiteko, funtsezkoa bilakatzen ari da bereizmen handiko teknikak garatzea. Egungo berrikuntzetako bat dimentsio biko kromatografiaren garapena da, modu horretan, dimentsio bakarreko kromatografiarekin bereizi ezinak diren konposatuak azter daitezkeelarik. Lan honetan, beraz, aztergai hartuko dira dimentsio biko gas-kromatografiaren ezaugarriak, abantailak eta geologia, ingurumena edo elikadura bezalako zientzia arlo batzuetako erabilerak