Enantioseparation and ecotoxicity evaluation of ibrutinib by Electrokinetic Chromatography using single and dual systems

In this work, two chiral methods enabling the separation of ibrutinib enantiomers were developed by Electrokinetic Chromatography. A cyclodextrin (CD) or a mixture of the CD and a chiral ionic liquid (CIL) was used as chiral selector. Using the single CD system, seven neutral and six anionic CDs were tested in a formate buffer at pH 3.0 working in positive and negative polarity, respectively. The use of sulfated-?-CD (S-?-CD) and negative polarity originated the best results considering analysis time and enantioresolution. The optimization of the experimental conditions allowed obtaining the separation of ibrutinib enantiomers in an analysis time of 4.2 min with an enantioresolution value of 1.5. The effect of the addition of fifteen CILs on the enantioresolution was evaluated showing that both analysis time and enantioresolution were generally increased. A mixture of S-?-CD and [TMA][L-Lys] was selected which provided the separation of ibrutinib enantiomers in 8.1 min with an enantioresolution value of 3.3 under the same experimental conditions as in the case of using the single CD system. The enantiomeric impurity (S-ibrutinib) was the first-migrating isomer when using the single CD and the combined CD/CIL systems, as corresponds to the most desirable situation. Both chiral methods allowed the detection of the enantiomeric impurity up to a 0.1 % as established by the International Council on Harmonization. After establishing the analytical characteristics of both chiral methodologies developed, they were applied to the enantiomeric determination of ibrutinib in a pharmaceutical formulation for hospital use marketed as pure enantiomer (R-ibrutinib) and to evaluate the stability and ecotoxicity of racemic ibrutinib and R-ibrutinib on Daphnia magna. The developed methodologies enabled, for the first time, the rapid chiral quantitation of ibrutinib in abiotic and biotic matrices

Enantiomeric separation of panthenol by Capillary Electrophoresis. Analysis of commercial formulations and toxicity evaluation on non-target organisms

The first CE methodology enabling the enantiomeric separation of panthenol was developed in this work. Electrokinetic chromatography with cyclodextrins (CD-EKC) was the CE mode employed for this purpose. The effect of different experimental variables such as the nature and concentration of the cyclodextrin, the temperature and the separation voltage was investigated. The best enantiomeric separation was obtained with 25 mM (2-carboxyethyl)-?-CD (CE-?-CD) in 100 mM borate buffer (pH 9.0), with a separation voltage of 30 kV and a temperature of 30?C. Under these conditions, an enantiomeric resolution of 2.0 in an analysis time of 4.2 min was obtained, being the biologically active enantiomer D-panthenol (dexpanthenol) the second-migrating enantiomer. The analytical characteristics of the method were evaluated in terms of precision, accuracy, selectivity, linearity, LOD, and LOQ, showing a good performance for the quantitation of dexpanthenol in cosmetic and pharmaceutical formulations. The enantiomeric impurity (L-panthenol) could be detected at a 0.1 % level with respect to the majority enantiomer, allowing to accomplish the requirements of the ICH guidelines. The method was also successfully applied to study the stability of panthenol under abiotic and biotic conditions and its toxicity on non-target organisms (the aquatic plant Spirodela polyrhiza)

Stereoselective separation of sulfoxaflor by electrokinetic chromatography and applications to stability and ecotoxicological studies

An Electrokinetic Chromatography method was developed for the stereoselective analysis of sulfoxaflor, a novel sulfoximine agrochemical with two chiral centers. A screening with fourteen negatively charged CDs was performed and Succinyl-?-CD (Succ-?-CD) was selected. A 15 mM concentration of this CD in a 100 mM borate buffer (pH 9.0), using an applied voltage of 20 kV and a temperature of 15 ?C made possible the baseline separation of the four stereoisomers of sulfoxaflor in 13.8 min. The evaluation of the linearity, accuracy, precision, LODs and LOQs of the method developed showed its performance to be applied to the analysis of commercial agrochemical formulations, the evaluation of the stability of sulfoxaflor stereoisomers under biotic and abiotic conditions, and to predict, for the first time, sulfoxaflor toxicity (using real concentrations instead of nominal concentrations), on two non-target aquatic organisms, the freshwater plant, Spirodela polyrhiza, and the marine bacterium, Vibrio fischer

A capillary micellar electrokinetic chromatography method for the stereoselective quantitation of bioallethrin in biotic and abiotic samples

A capillary micellar electrokinetic chromatography (MEKC) method was developed enabling the stereoselective separation of the insecticide bioallethrin. The use of sodium deoxycholate bile salt and acetyl-beta-cyclodextrin (acetyl-beta-CD) made possible the separation of bioallethrin stereoisomers with a high enantioresolution (7.4) in a short analysis time (6.5 min). The analytical characteristics of the developed method were evaluated in terms of linearity, accuracy, precision, and limits of detection (LOD) and quantitation (LOQ) showing a good performance for the quantitation of bioallethrin stereoisomers with LODs of 0.2 and 0.3 mg/L. The developed method was applied to the stereoselective analysis of a commercial bioallethrin pediculicide formulation and to evaluate the toxicity of bioallethrin stereoisomers on the growth of the unicellular freshwater green alga Pseudokirchneriella subcapitata and on the germination of the higher plant Sorghum bicolor (non-target organisms). The analysis of the commercial pediculicide showed a good agreement between the contents determined for the two stereoisomers and those labelled in the commercial samples. Different toxic responses and biodegradation profiles were found for each stereoisomer in ecotoxicity assays. The mixture of SIR stereoisomers of bioallethrin resulted more toxic than S-bioallethrin for green algae, with EC50 values of 1.10 +/- 0.06 for the mixture and of 1.73 +/- 0.05 mg/L for the pure S-biallethrin (esbiol). Germination of plants seeds was also affected. (C) 2017 Elsevier B.V. All rights reserved

Effect of Carbamazepine, Ibuprofen, Triclosan and Sulfamethoxazole on Anaerobic Bioreactor Performance: Combining Cell Damage, Ecotoxicity and Chemical Information

Pharmaceuticals and personal care products (PPCPs) are partially degraded in wastewater treatment plants (WWTPs), thereby leading to the formation of more toxic metabolites. Bacterial populations in bioreactors operated in WWTPs are sensitive to different toxics such as heavy metals and aromatic compounds, but there is still little information on the effect that pharmaceuticals exert on their metabolism, especially under anaerobic conditions. This work evaluated the effect of selected pharmaceuticals that remain in solution and attached to biosolids on the metabolism of anaerobic biomass. Batch reactors operated in parallel under the pressure of four individual and mixed PPCPs (carbamazepine, ibuprofen, triclosan and sulfametoxazole) allowed us to obtain relevant information on anaerobic digestion performance, toxicological effects and alterations to key enzymes involved in the biodegradation process. Cell viability was quantitatively evaluated using an automatic analysis of confocal microscopy images, and showed that triclosan and mixed pollutants caused higher toxicity and cell death than the other individual compounds. Both individual pollutants and their mixture had a considerable impact on the anaerobic digestion process, favoring carbon dioxide production, lowering organic matter removal and methane production, which also produced microbial stress and irreversible cell damage.Comunidad de MadridUniversidad de Alcal

Membranas electrohiladas de doble acción para tratamiento de agua

Número de publicación: 2 663 129 Número de solicitud: 201600852 51 Int. CI.: B01D 61/00 (2006.01) C02F 1/44 (2006.01)Membranas electrohiladas de doble acción para tratamiento de agua. La presente invención consiste en un procedimiento para la fabricación de membranas activas basadas en fibras submicrométricas que combinan una acción antimicrobiana con la capacidad de retención de contaminantes apolares en solución acuosa. Las membranas se producen mediante un procedimiento de electrohilado en disolución acuosa a partir de mezclas de un poliácido y un polialcohol solubles en agua que se estabilizan mediante un procedimiento de curado y se post-funcionalizan mediante la incorporación de dendrímeros con terminación amino mediante un procedimiento de injertado can ayuda de un agente de acoplamiento. La aplicación del material es la producción de membranas o componentes de membranas multicapa para tratamiento de agua con acción antimicrobiana y con capacidad para retener contaminantes apolares.Universidad de Almerí

Restructuración de asignaturas de Ingeniería Química para su adaptación al EEES mediante la utilización de TIC

Este trabajo aborda la reestructuración de las asignaturas de Ingeniería Química impartidas en dos licenciaturas de la Universidad de Alcalá para su adaptación al EEES. Mediante la utilización intensiva de TIC en el desarrollo de la enseñanza semipresencial, se han rediseñado estas asignaturas orientándolas para favorecer el aprendizaje autónomo y colaborativo y mejorar los canales de comunicación del binomio profesor-alumno. Para ello y utilizando como apoyo la plataforma virtual de la Universidad de Alcalá y una plataforma pública de acceso restringido, se han desarrollado una serie de actividades que incluyen la elaboración de bitácoras grupales y la técnica de enseñanza basada en la resolución de problemas (PBL)

Enzyme response of activated sludge to a mixture of emerging contaminants in continuous exposure.

The relevant information about the impacts caused by presence of emerging pollutants in mixtures on the ecological environment, especially on the more vulnerable compartments such as activated sludge (AS) is relatively limited. This study investigated the effect of ibuprofen (IBU) and triclosan (TCS), alone and in combination to the performance and enzymatic activity of AS bacterial community. The assays were carried out in a pilot AS reactor operating for two-weeks under continuous dosage of pollutants. The microbial activity was tracked by measuring oxygen uptake rate, esterase activity, oxidative stress and antioxidant enzyme activities. It was found that IBU and TCS had no acute toxic effects on reactor biomass concentration. TCS led to significant decrease of COD removal efficiency, which dropped from 90% to 35%. Continuous exposure to IBU, TCS and their mixtures increased the activities of glutathione s-transferase (GST) and esterase as a response to oxidative damage. A high increase in GST activity was associated with non-reversible toxic damage while peaks of esterase activity combined with moderate GST increase were attributed to an adaptive response