Implementing the Use of Collision Cross Section Database for Phycotoxin Screening Analysis

The increased consumption of blue-green algae (BGA)-based dietary supplements has raised concern about their food safety, especially about cyanotoxin presence. The hyphenation of liquid chromatography with ion mobility mass spectrometry represents a relevant tool to screen several compounds in a large variety of food matrices. In this work, ultrahigh-performance liquid chromatography coupled to traveling wave ion mobility spectrometry/quadrupole time-of-flight mass spectrometry (UHPLC-TWIMS-QTOF) was employed to establish the first comprehensive TWIMS-derived collision cross section database (TWCCSN2) for phycotoxins. The database included 20 cyanotoxins and 1 marine toxin. Accurate m/z, retention times, and TWCCSN2 values were obtained for 81 adducts in positive and negative electrospray (ESI+/ESI–) modes. Reproducibility and robustness of the TWCCSN2 measurements were determined to be independent of the matrix. A screening was carried out on 19 commercial BGA dietary supplements of different composition. Cyanotoxins were confidently identified in five samples based on retention time, m/z, and TWCCSN2.The University of Parma through the action Bando di Ateneo 2021MUR-Italian Ministry of Universities and Research-D.M. 737/2021-PNR-PNRR−NextGenerationEU, (ii) from the Project PID2021-127804OB-I00Spanish MCIN/AEI/10.13039/501100011033ERDF A way of making Europe” and from the Andalousian Government (Project ref. PROYEXCEL_00195)The Grant (FPU17/03810) financed by MCIN/AEI/ 10.13039/501100011033, by “ESF Investing in your future”.Grant IJC2019-040989-I funded by MCIN/AEI/10.13039/501100011033Waters Italy for providing the Atlantis Premier BEH Z-HILIC colum

Multiclass cyanotoxin analysis in reservoir waters: tandem solid-phase extraction followed by zwitterionic hydrophilic interaction liquid chromatography-mass spectrometry

The presence of cyanobacteria and cyanotoxins in all water bodies, including ocean water and fresh water sources, represents a risk for human health as eutrophication and climate change are enhancing their level of proliferation. For risk assessment and studies on occurrence, the development of reliable and sensitive analytical approaches able to cover a wide range of cyanotoxins is essential. This work describes the development of an HILIC-MS/MS multiclass method for the simultaneous analysis of eight cyanotoxins in reservoir water samples belonging to three different classes according to their chemical structure: cyclic peptides (microcystin-LR, microcystin-RR and nodularin), alkaloids (cylindrospermopsin, anatoxin-a) and three non-protein amino acids isomers such as β-methylamino-L-alanine, 2,4-diaminobutyric acid and N-(2-aminoethyl)glycine). A SeQuant ZIC-HILIC column was employed to achieve the chromatographic separation in less than 12 min. Previously, a novel sample treatment based on a tandem solid-phase extraction (SPE) system using mixed cation exchange (MCX) and Strata-X cartridges was investigated with the aim of extracting and preconcentrating this chemically diverse group of cyanotoxins. The Strata-X cartridge, which was configured first in the line of sample flow, retained the low polar compounds and the MCX cartridge, which was at the bottom of the dual system, retained mainly the non-protein amino acids. The optimization procedure highlighted the importance of sample ion content for the recoveries of some analytes such as the isomers β-Nmethylamino-L-alanine and 2-4-diaminobutyric acid. Method validation was carried out in terms of linearity, limit of detection (LOD) and quantification (LOQ), recoveries, matrix effect and precision in terms of repeatability and intermediate precision. This work represents the first analytical method for the simultaneous analysis of these multiclass cyanotoxins in reservoir water samples, achieving LOQs in the very low range of 7·10-3 – 0.1 µg·L-1. Despite high recoveries obtained at the LOQ concentration levels (101.0-70.9%), relative standard deviations lower than 17.5% were achieved.RTI2018-097043-B-I00 financed by MCIN/ AEI /10.13039/501100011033/ FEDER “Una manera de hacer Europa”Spanish Network of Excellence in Sample preparation (RED2018-102522-T)FPU17/0381

Determination of Multiclass Cyanotoxins in Blue-Green Algae (BGA) Dietary Supplements Using Hydrophilic Interaction Liquid Chromatography-Tandem Mass Spectrometry

In recent years, the consumption of blue-green algae (BGA) dietary supplements is increasing because of their health benefits. However, cyanobacteria can produce cyanotoxins, which present serious health risks. In this work we propose hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry (HILIC-MS/MS) to determine cyanotoxins in BGA dietary supplements. Target toxins, including microcystin-leucine-arginine (MC-LR) and microcystin-arginine-arginine (MC-RR), nodularin, anatoxin-a and three non-protein amino acids, β-N-methylamino-L-alanine (BMAA), 2,4-diaminobutyric acid (DAB) and N-(2-aminoethyl)glycine (AEG), were separated using a SeQuant ZIC-HILIC column. Cyanotoxin extraction was based on solid–liquid extraction (SLE) followed by a tandem-solid phase extraction (SPE) procedure using Strata-X and mixed-mode cation-exchange (MCX) cartridges. The method was validated for BGA dietary supplements obtaining quantification limits from 60 to 300 µg·kg−1. Nine different commercial supplements were analyzed, and DAB, AEG, and MCs were found in some samples, highlighting the relevance of monitoring these substances as precaution measures for the safe consumption of these products

Determination of Multiclass Cyanotoxins in Blue-Green Algae (BGA) Dietary Supplements Using Hydrophilic Interaction Liquid Chromatography-Tandem Mass Spectrometry

In recent years, the consumption of blue-green algae (BGA) dietary supplements is increasing because of their health benefits. However, cyanobacteria can produce cyanotoxins, which present serious health risks. In this work we propose hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry (HILIC-MS/MS) to determine cyanotoxins in BGA dietary supplements. Target toxins, including microcystin-leucine-arginine (MC-LR) and microcystin-arginine-arginine (MC-RR), nodularin, anatoxin-a and three non-protein amino acids, beta-N-methylamino-L-alanine (BMAA), 2,4-diaminobutyric acid (DAB) and N-(2-aminoethyl)glycine (AEG), were separated using a SeQuant ZIC-HILIC column. Cyanotoxin extraction was based on solid-liquid extraction (SLE) followed by a tandem-solid phase extraction (SPE) procedure using Strata-X and mixed-mode cation-exchange (MCX) cartridges. The method was validated for BGA dietary supplements obtaining quantification limits from 60 to 300 mu g center dot kg(-1). Nine different commercial supplements were analyzed, and DAB, AEG, and MCs were found in some samples, highlighting the relevance of monitoring these substances as precaution measures for the safe consumption of these products.MCIN/ AEI RTI2018-097043-B-I00Project Junta de Andalucia-Programa Operativo FEDER B-AGR-202-UGR20MCIN/AEI and FSE FPU17/0381

Evaluación formativa ¿una realidad utópica?

La evaluación condiciona poderosamente los procesos de aprendizaje del alumnado y ninguna innovación docente será efectiva si no va acompañada de innovaciones en el modo de concebirla. Creemos que la forma más adecuada de abordar esta tarea consiste en hacer de la evaluación un instrumento de aprendizaje. En esta comunicación presentamos la experiencia de un Equipo Docente de la Universidad de Granada, constituido por profesorado experimentado y principiante, en el que se han llevado a cabo una serie de acciones dirigidas a la formación, reflexión y puesta en práctica de estrategias de Evaluación formativa y compartida que nos permitan avanzar en el sentido propuesto. Entre los resultados obtenidos destacamos la experiencia de formación y reflexión sobre la labor docente dentro de un grupo de trabajo cooperativo que sirve como punto de referencia tanto a los profesores noveles como a los experimentados. Por otra parte, se están realizando innovaciones en evaluación en asignaturas de características muy diversas pertenecientes a diferentes titulaciones.SIN FINANCIACIÓNNo data 201

La evaluación formativa y compartida como aspecto fundamental en la formación del profesorado novel universitario: experiencia en las Facultades de Ciencias y Farmacia de la Universidad de Granada

We present the experience of a teaching team at the University of Granada made up of five experienced teachers and thirteen novices all working in the areas of Health Sciences and Experimental Sciences. This experience involved processes of training, self-criticism and putting into practice some strategies aimed at improving the teaching-learning process. In this article the following points are covered: The background of the team and the current situation, specifically the activities carried out and the results obtained with respect to the novice teachers. Among the developments we can point out innovations in Formative and Shared Evaluation in diverse subjects within the departments of Fine Arts, Biology, Environmental Science, Pharmacy, Chemical Engineering, and Chemistry. The experience of the teaching team as a collaborative workgroup is useful not only to the novice teachers but also to the experienced teachers.Se presenta la experiencia de un equipo docente de la Universidad de Granada, constituido por cinco profesores experimentados y trece principiantes pertenecientes a las áreas de ciencias experimentales y de la salud. En dicha experiencia se han llevado a cabo una serie de acciones de formación, reflexión y puesta en práctica de estrategias dirigidas a la mejora del proceso de enseñanzaaprendizaje. En este artículo se detallan: los antecedentes del equipo, sus intereses e inquietudes y la situación actual especificando las actividades realizadas y los resultados obtenidos en el trabajo desarrollado con el profesorado principiante. Entre las tareas desarrolladas podemos destacar las innovaciones realizadas en evaluación formativa y compartida en asignaturas de características muy diversas, pertenecientes a las titulaciones de Bellas Artes, Biología, Ciencias Ambientales, Farmacia, Ingeniería Química y Química. Asimismo la experiencia del equipo como grupo de trabajo cooperativo ha servido de punto de referencia tanto a los profesores noveles como a los experimentados