Aresatz Usobiaga's research while affiliated with Universidad del País Vasco / Euskal Herriko Unibertsitatea and other places

Publications (60)

Article
The determination of the concentration of endocannabinoids and related compounds in human plasma has become a matter of interest due to their implication in physiological processes and, thus, their possible relation with physiological conditions or illnesses. The analysis of these compounds though has to be carefully designed as they are found in v...
Article
Full-text available
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 e...
Article
Metabolomics as a diagnosis tool for plant performance has shown good features for breeding and crop improvement. Additionally, due to limitations in land area and the increasing climate changes, breeding projects focusing on abiotic stress tolerance are becoming essential. Nowadays no universal method is available to identify predictive metabolic...
Chapter
The cannabis industry is undergoing a significant change due to the legalization in many countries. This makes it necessary to introduce standard procedures and regulations on the quality of consumer products regarding bioactive compounds. Thus, it is essential to provide reliable and robust analytical tools for the analysis of the content of canna...
Article
This work describes the analysis of both target and non-target compounds in paper and cardboard materials together with the characterization of their migration to Tenax® by means of liquid chromatography coupled to both low (LC-QqQ) and high resolution tandem mass spectrometry (LC-q-Orbitrap), respectively. To this aim, an entire analytical procedu...
Article
In this work, the full optimisation and validation procedure to analyse a wide set of emerging organic contaminants in biotissues (mussel and fish muscle, liver, gills and brain) and biofluids (fish plasma and bile) is described. The target families include artificial sweeteners, industrial products, hormones, pharmaceutical and personal care produ...
Article
The extensive use of the organic UV filter oxybenzone has led to its ubiquitous occurrence in the aquatic environment, causing an ecotoxicological risk to biota. Although some studies reported adverse effects, such as reproductive toxicity, further research needs to be done in order to assess its molecular effects and mechanism of action. Therefore...
Article
The calibration of two passive samplers for the determination of 20 emerging organic compounds in seawater is described in this work: i) a new version of polar organic chemical integrative sampler (POCIS) containing 100 mg of mixed-mode anion exchanger (Strata X-AW) and 100 mg of polymeric HLB (Plexa) sorbent materials and using a highly porous Nyl...
Article
This work describes the optimization, validation, and application in real samples of accurate and precise analytical methods to determine ten fluoroquinolones (FQs) (norfloxacin, enoxacin, pefloxacin, ofloxacin, levofloxacin, ciprofloxacin, danofloxacin, lomefloxacin, enrofloxacin, and sparfloxacin) in different environmental matrices, such as wate...
Article
Full-text available
Tesi hau bi zutabe nagusitan banatzen da. Lehenengoan ardo hondakinen balioa handitzeko metodologia bat garatu genuen. Lehenik, ardo hondakinetatik polifenolak eta gantz azidoak bakoitza bere aldetik erauzi genituen jariakin gainkritikoak erabiliz. Polifenolak ez dira oso egonkorrak ordea eta gorputzean bioeskuragarritasun baxua dute. Arazo hauek k...
Article
Full-text available
A high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) method for simultaneous quantification of Δ9-tetrahydrocannabinol (THC), its two metabolites 11-hydroxy-Δ9-tetrahydrocannabinol (11-OH-THC) and 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THC-COOH), and four additional cannabinoids (cannabidiol (CBD), cannabiger...
Article
Full-text available
Laburpena: Etorkizun hurbilean kannabisa sendagai bezala erabili ahal izateko bi urrats eman dira lan honetan. Alde batetik, landareak euren efektu fisiologikoekin lotzeko lagungarria izan daitekeen kannabinoideen hatz-marka ikertzeko metodo bat garatu da fragmentazio bikoitzeko masa-espektometriari akoplaturiko eraginkortasun handiko likido kromat...
Article
Full-text available
The evolution of major cannabinoids and terpenes during the growth of Cannabis sativa plants was studied. In this work, seven different plants were selected: three each from chemotypes I and III and one from chemotype II. Fifty clones of each mother plant were grown indoors under controlled conditions. Every week, three plants from each variety wer...
Article
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Laburpena: Lan honetan, optimizatu egin da bi urratseko jariakin gainkritikoaren bi-dezko erauzketa (SFE Supercritical Fluid Extraction), ardo hondakinetatik konposatu bioaktiboak lortzeko. Ondorioz, lortu da lehen urratsean gantz azidoak soilik eta biga-rren urratsean polifenolak soilik erauztea. Polifenolek egonkortasun eskasa dute ordea. Hori de...
Article
The interest in the analysis of alkylphenols (APs) has widely increased in the last decades because of the endocrine disrupting features of these phenol derivatives. However, the isolation and identification of many of the multiple chemical structures of all APs is a very challenging task because of their similar physicochemical properties. In this...
Article
Full-text available
In this study, supercritical fluid extraction has been successfully applied to a sequential fractionation of fatty acids and polyphenols from wine wastes (2 different vitis vinifera grapes). To this aim, in a 1st step just fatty acids were extracted and in a 2nd one the polyphenols. The variables that affected to the extraction efficiency were sepa...
Article
Full-text available
High performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) has been successfully applied to cannabis plant extracts in order to identify cannabinoid compounds after their quantitative isolation by means of supercritical fluid extraction (SFE). MS conditions were optimized by means of a central composite design (CCD) approach, and...
Article
In this work, home-made Polar Organic Chemical Integrative Samplers (POCIS) were studied for passive sampling of 15 endocrine disrupting compounds (4 alkylphenols and steroid hormones) in influent and effluent samples of wastewater treatment plants (WWTPs) as well as up- and downstream of the receiving river water. POCIS calibration at laboratory c...
Article
In the present work the simultaneous extraction for the multiresidue determination in wastewater samples of organic compounds such as polychlorinated biphenyls (PCBs), polybrominated biphenyls (PBBs), pesticides, polycyclic aromatic hydrocarbons (PAHs), phthalate esters (PEs), alkylphenols (APs), bisphenol A (BPA) or hormones included in different...
Chapter
The European Water Framework Directive 2000/60 is one of the key legislations introduced for many years in water management and protection fields. The model of water management established by this directive is the river basin. There are a variety of indicators to define the good ecological and chemical status, including a list of priority and emerg...
Article
In the present work, the separation of complex nonylphenol technical mixtures has been optimized using comprehensive two-dimensional gas chromatography coupled with a flame ionization detector and quadrupole mass spectrometer (GC×GC-qMS), using valve-based modulator. The optimization of GC×GC-qMS has been carried out using experimental designs and...
Article
Large volume injection-programmable temperature vaporization-gas chromatography-mass spectrometry (LVI-PTV-GC-MS) was optimized for the determination of estrone (E1), 17β-estradiol (E2), 17α-ethynyl estradiol (EE2), mestranol (MeEE2) and estriol (E3) for their determination in environmental samples (estuarine water, wastewater, fish bile and fish h...
Article
Full-text available
According to the European Water Framework Directive (WFD), alkylphenols, such as octylphenols and nonylphenols, and 17β-oestradiol are considered as priority or emerging pollutants, respectively, mainly due to their possible properties as endocrine-disrupting compounds (EDCs). EDCs are accumulated in liver, fat, kidney and bile in the glucuronide f...
Article
The determination of target analytes such as nonyl- and octylphenols and 17beta-estradiol in fish homogenate require of solid-liquid extraction step. In this work microwave-assisted extraction (MAE) and focused-ultrasound liquid extraction (FUSLE) were studied as two different alternatives for extraction of the target compounds in zebrafish (Danio...
Article
Full-text available
Polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), methylmercury (MeHg) and butyltins (mono-, di- and tri-butyltin, MBT, DBT and TBT) were monitored in oysters (Crassostrea sp.) and sediments collected in different sampling points of the UNESCO reserve of the biosphere of Urdaibai (Bay of Biscay) from March 2006 to June 2007...
Article
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Mussels are used as bioindicators of chemical pollution in coastal and estuarine waters. We measured the concentrations of polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), phthalate esters (PEs), butyltins, and metals (Cd, Co, Cr, Cu, Hg, Mn, Ni, Pb, V, and Zn) in mussel tissues collected from the lower Bilbao estuary (Arr...
Article
Introduced in 1999 as a novel solventless sample preparation method, stir-bar sorptive extraction (SBSE) has become a popular analytical technique for the pre-concentration of organic compounds into a polydimethylsiloxane (PDMS)-coated stir-bar. In the last 10 years, hundreds of applications in the environmental, food and biomedical fields can be f...
Article
Cup horn boosters are miniaturized ultrasound baths that maximize efficiency and precision. The optimization of an ultrasonic-assisted derivatization step by means of a cup horn booster and the determination of estrone, 17beta-estradiol, estriol, 17alpha-ethynyl estradiol and mestranol was developed by GC-MS. Different derivatization reagents and s...
Article
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The paper presents the first comprehensive account of congener profiles of polycyclic aromatic hydrocarbons (PAHs) in intertidal bivalve mollusks [Meretrix meretrix, Macoma birmanica, and Sanguilonaria (Soletellina) acuminata] of Sunderban mangrove wetland (India). The main aim of this work was to use the bivalves as bioindicators of the contaminat...
Article
In this work the simultaneous purge-and-trap (P&T) preconcentration of volatile fatty acids (acetic acid, propanoic acid, butanoic acid, iso-butanoic acid, pentanoic acid, iso-pentanoic acid, hexanoic acid and heptanoic acid), phenols (phenol, 4-methylphenol and 4-ethylphenol) and indoles (indole and 3-methylindole) from cow slurries was carried ou...
Article
Stir bar soptive extraction (SBSE) coupled to thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) and membrane-assisted solvent extraction (MASE) coupled to large volume injection-programmed temperature vaporisation-GC-MS (LVI-PTV-GC-MS) were optimised for the simultaneous determination of polycyclic aromatic hydrocarbons (PAHs), pol...
Article
Focused ultrasonic solid-liquid extraction (FUSLE) has been optimised for simultaneous analysis of polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), phthalate esters (PEs), and nonylphenols (NPs) in sediment samples. Optimisation was performed using naturally polluted freeze-dried sediment samples. The variables studied dur...
Article
Full-text available
Along 10 campaigns, from June 2002 to September 2004, the concentrations of 16 polycyclic aromatic hydrocarbons (PAHs) were measured in sediments and oysters (Crassostrea sp.) taken from four sites in the Unesco protected natural reserve of Urdaibai (Basque Country, Bay of Biscay). Total PAH concentration ranged from 0.7 to 140 microg kg(-1) (dw) i...
Article
Thermodynamic and Raman spectroscopic speciation was used to define the operating conditions for an innovative cleaning treatment of the decayed carbonate-based stones using ion exchange technology. The conditioning process of the Lewatit OC1071 anion exchanger with EDTA (Y) was monitored by ionic chromatography. Characterisation of the initial (R-...
Article
In this work, making use of experimental designs, headspace-stir bar sorptive extraction (HS-SBSE) followed by thermal desorption (TD) coupled to a gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of mercury and tin organometallic compounds present in surface water, sediment and biological tissue was optimized. All so...
Article
Headspace solid-phase microextraction was optimised for the simultaneous preconcentration of methylmercury (MeHg+), monobutyltin, dibutyltin, tributyltin, monophenyltin (MPhT), diphenyltin (DPhT), and triphenyltin (TPhT) from sediments and biota. Extraction time (3-24 min), extraction temperature (20-90 degrees C), desorption time (1-10.4 min), des...
Article
A method for the determination of polybrominated diphenyl ethers (PBDEs) and polybrominated biphenyls (PBBs) in water samples is proposed. The method involving stir bar sorptive extraction (SBSE) and thermal desorption followed by gas chromatography coupled with mass spectrometry was optimised using statistical design of experiments. In the first p...
Article
Stir bar sorptive extraction (SBSE) and thermal desorption followed by capillary gas chromatography coupled to mass spectrometry (SBSE-TD-GC-MS) was applied to the simultaneous determination of ultra-traces of 16 polycyclic aromatic hydrocarbons (PAHs), 12 polychlorinated biphenyls (PCBs), 6 phthalate esters (PEs) and 3 nonylphenols (NPs) in water...
Article
Composition of moonmilk deposits located in different zones of the tourist Dolomite Cave of Pozalagua (Karrantza, Basque Country, North of Spain) was established by Raman spectroscopy. The deposits were located in column bases and detached rocks near a gour full of water or a dripping zone. Hydromagnesite (Mg(5)(CO(3))(4)(OH)(2).4H(2)O) with a stro...
Article
The on-fibre derivatisation of volatile fatty acids (VFAs) using N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA) was optimised in the simultaneous determination of VFAs together with phenols and indoles by headspace solid-phase microextraction (SPME)-gas chromatography-mass spectrometry. Firstly, the nature of the SPME fibre was op...
Article
Odorous organic compounds from liquid and gas samples of animal wastes were studied by headspace (HS)-solid-phase microextraction (SPME)-GC-MS. 1-Pirenyldiazomethane (PDAM) was adsorbed/absorbed on the SPME fibre in order to obtain the corresponding ester derivatives during the preconcentration step. The SPME fibre was immersed into a PDAM solution...
Article
This work was conducted to study a new separation and evaluation approach for the chemical fingerprinting of petroleum biomarkers in biota samples. The final aim of this work was to study the correlation between the observed effects in the shore habitats (mussels and limpets) and one pollution source: the oil spill of the Prestige tanker. The metho...
Article
A simple, fast, and accurate method for the simultaneous determination of methylmercury (MeHg(+)), monobutyltin (MBT), dibutyltin (DBT) and tributyltin (TBT) in seafood is proposed. The method makes use of relatively cheap instrumentation and allows simultaneous analysis of those four species in a routine basis. The sample is treated with methanoli...
Article
Microwave-assisted extraction (MAE) of nonylphenols (NP), nonylphenol mono- and diethoxylates (NP1EO and NP2EO, respectively) and phthalate esters was optimised using an experimental design approach. A D-optimal mixture design was used to optimise the pressure inside the extraction vessel (110–207kPa), the extraction time (5–25min) and the extracti...
Article
Full-text available
A new method was developed for the simultaneous extraction of polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), phthalate esters (PEs), nonylphenols (NPs) and nonylphenol mono- and diethoxylates (NP1EOs and NP2EOs, respectively) in sediment samples by means of a closed microwave system. The extractions were carried out at 2...
Article
The electrical conductivity of H2TiF6 (1) + HF (2) + H2O (3) mixtures was measured in a wide range of mass fractions (0% < w1 < 55% and 0% < w2 < 11%) and temperature (15 °C < t < 35 °C) by means of an automatic system based on the “electrodeless conductivity” technique. The results were fitted to a polynomial equation in w1, w2, and t using a Math...
Article
A MATHEMATICA package, 'CONDU.M', has been developed to find the polynomial in concentration and temperature which best fits conductimetric data of the type (kappa, c, T) or (kappa, c1, c2, T) of electrolyte solutions (kappa: specific conductivity; ci: concentration of component i; T: temperature). In addition, an interface, 'TKONDU', has been writ...
Article
Different aspects of the conductivity of concentrated electrolyte solutions and their application to design and control of chemical processes are discussed and reviewed, with particular focus on the work of our research group during the last few years. An automated system based on the electrodeless conductivity technique for the measurement of the...
Article
The electrical conductivity of the HCl + KCl + H2O ternary system has been measured in a wide range of compositions (0 mol.dm(-3) < c(HCl) < 6 mol.dm(-3) and 0 mol.dm(-3) < c(KCl) < 1.2 mol.dm(-3)) and temperatures (15 degrees C < t < 45 degrees C) making use of an automated station for conductometric titration based on the "electrodeless conductiv...
Article
A critical comparison among models to fit conductimetric data of 1:1 strong electrolyte solutions was carried out. The most reliable experimental results of conductimetric measurements in aqueous media at 25°C up to quite high concentrations, e.g. 4–5 mol dm−3 reported in the literature were considered. The models included in the study are empirica...
Article
A modification of the Falkenhagen equation is proposed, which fits correctly data of 29 different 1:1 aqueous electrolyte solutions up to very high concentrations. The concept of activity is used to account for deviations from ideality appearing at higher concentrations. A discussion about trends in the value of the 'distance of closest approach be...

Citations

... For the same reason, using the ionic gelation process, Taghiloo, S. et al. developed sodium alginate and chitosan nanoparticles that contained Echinacea angustifolia extract to increase their stability and prolong their release [40]. Using the vibration microencapsulation nozzle technique, Villate, A. et al. synthetized chitosancoated alginate microcapsules, which contained Cannabis raw extract, to obtain an edible pharmaceutical-grade product [41]. In contrast, our study used microencapsulation technology to ensure the release of the RG plant extract into the intestine, minimizing the effect of acidic pH on the bioactivity of the compounds. ...
... Oxybenzone poses a threat to crop yield for a variety of crops, regardless of whether the cultivation systems use hydroponic methods, irrigation using R1 water (recycled waters from sewage/waste waters treatment facilities), or amended soils human or livestock biosolids (Cabrera-Peralta and Peña-Alvarez, 2018;Ramos et al., 2021;Gautam et al., 2022). By understanding the homeostatic and metabolic processes susceptible to oxybenzone toxicity, we can select for genotypic markers that can give these susceptible crops an advantage against the ubiquitous exposure to oxybenzone (Villate et al., 2021). A multi-array 'omics' approach is being used to successfully accelerate the selection and cultivation of stress tolerant plants (Razzaq et al., 2019;Tahir ul Qamar et al., 2020;Pandey et al., 2021;Zhang et al., 2022). ...
... After that GC-MS is conveyed for the examination of cannabinol, cannabidiol, and different constituents of cannabis. [67] Narcotics and psychoactive drugs are identified from human urination and plasma samples which are separated by SUPRAS (Supramolecular Solvent) method. It is a valuable method in clinical and criminological cases in narcotics and psychoactive drug misuse. ...
... Stir bar sorptive extraction (SBSE) was first described by Baltussen in 1999 [75]. The method was proposed as a solvent-free sample enrichment technique that combines extraction and preconcentration of the target analytes. ...
... ( Fig. S3), was identified in the samples examined herein. This substance is known as an antioxidant and stabilizer in polymers employed in food manufacturing [61], and is widely used to prevent free-radical-mediated oxidation in fluids (e.g., fuels and oils) and other materials [62]. It is reported that 2,6-di-tert-butyl-4-ethylphenol not only hinders the survival and reproduction of aquatic organisms, but also endangers human health [63,64]. ...
... Regarding the extraction step, most of the protocols developed for multiresidue trace determination of pharmaceuticals in fish are based on ACN or MeOH as extraction solvents [11,21], with a predominant use of neutral [22,33,34] and acidified solvents [26,27,35]. However, to the best of our knowledge, basified solvents have not yet been systematically evaluated and applied for this purpose in the literature. ...
... Furthermore, fatty acids were down-regulated in the LT-28d samples, whereas, triglyceride was up-regulated, suggesting triglyceride accumulation in the liver and subsequently an increase in intrahepatic lipids. Lipid alterations in fish have been associated with xenobiotic exposure, including carbendazim (Ezeoyili et Sakr & Shalaby, 2014;Ziarrusta et al., 2018). A study carried out on adult zebrafish showed that carbendazim exposure affected glycolipid metabolism and detoxification metabolism in the liver (Bao et al., 2020). ...
... Other resin sorbents studies for detecting pharmaceutical and pesticides in river and ground water, have used Strata-X using a nylon Membrane and mixed Polymer Sampler (MPS) [248][249][250][251]. A copolymer of poly(divinylbenzene)-N-vinylpyrrolidone was used as resin sorbent for monitoring 46 pesticides, 17 pharmaceuticals and some artificial sweeteners [252]. ...
... The quantification of the investigated pharmaceuticals in various sample forms was carried out using a variety of analytical techniques, such as spectrofluorimetry [6,7], highperformance liquid chromatography (HPLC) [8][9][10][11], and liquid chromatography coupled to a mass spectrometric detector (LC-MS/MS) [12,13]. The extensive usage of FQs in recent years has raised concerns for people since they have a detrimental impact on them. ...
... Modulation of the endocannabinoid system by targeting G-protein-coupled cannabinoid receptors has broad therapeutic applications ranging from pain to cancer treatment [27,28]. A series of oxazolo [5,4-d]pyrimidines (22) were designed via the bioisosterism strategy as new cannabinoid receptor 1 (CB 1 R) and cannabinoid receptor 2 (CB 2 R) modulators ( Figure 5) [29]. ...