Efficient Validation Strategies in Environmental Analytical Chemistry: A Focus on Organic Micropollutants in Water Samples

This article critically reviews analytical method validation and quality control applied to the environmental chemistry field. The review focuses on the determination of organic micropollutants (OMPs), specifically emerging contaminants and pesticides, in the aquatic environment. The analytical technique considered is (gas and liquid) chromatography coupled to mass spectrometry (MS), including high-resolution MS for wide-scope screening purposes. An analysis of current research practices outlined in the literature has been performed, and key issues and analytical challenges are identified and critically discussed. It is worth emphasizing the lack of specific guidelines applied to environmental analytical chemistry and the minimal regulation of OMPs in waters, which greatly affect method development and performance, requirements for method validation, and the subsequent application to samples. Finally, a proposal is made for method validation and data reporting, which can be understood as starting points for further discussion with specialists in environmental analytical chemistry.D.F.-S. acknowledges the Ministerio de Universidades in Spain for his Margarita Salas postdoctoral grant (Ref. MGS/2021/15). The authors from University Jaume I acknowledge financial support from Generalitat Valenciana (Research Group of Excellence Prometeo 2019/040) and Ministerio de Ciencia e Innovación (Ref. PID2021-127451OB-I00). J.B.Q. acknowledges funding provided by Xunta de Galicia (Ref. ED431C 2021/06), the Spanish Agencia Estatal de Investigación – MCIN/AEI/10.13039/501100011033 (Ref. PID2020-117686RB-C32).S

Contribution to the knowledge of the parasitic trematodes of «thrushes» in Granada (Spain)

Se está llevando a cabo un estudio sobre la helmintofauna parásita de aves pertenecientes al género Turdus «zorzales » ( T. philomelos, T. iliacus, T. viscivorus y T. merula). En este trabajo se denuncia, por primera vez en nuestro país, el trematodo Cyclocoelum mutabile en los sacos aéreos de Turdus philomelos (zorzal común) y se realiza una breve descripción de su morfología.A stady is being carried out on the parasitic helminthfauna in birds belonging to the genus Turdus «thrushes» (T. philomelos, T. iliacus, T, viscivorus y T. merula). In this article is noticed, the trematode Cyclocoelum mutabile, parasite of air sacs of Turdus philomelos (common thrush). For the first time in Spain, also, a brief morphological description is made

Reverse Trojan-horse effect decreased wastewater toxicity in the presence of inorganic nanoparticles

We studied the toxicological interaction of 46 micropollutants from a biologically treated wastewater effluent in mixtures with silica, amine-modified silica, titanium dioxide and magnetite nanoparticles. The pollutants tracked in this work were polar pharmaceuticals belonging to different therapeutic groups, some of their metabolites and artificial sweeteners, the concentrations of which were mostly in the tens to hundreds of ng L-1 range. The results showed particularly high adsorption for furosemide, gemfibrozil and the aminopyrine metabolite 4FAA. There was preferential adsorption of the less polar compounds on the less polar nanoparticles. The total amounts of compounds adsorbed and quantified were 13.4, 4.8, 10.8 and 7.1 μg g-1 for SiO2, SiO2-NH2, TiO2 and Fe3O4, respectively. The toxicity of wastewater-nanoparticle mixtures was assessed using the bioluminescent cyanobacterium Anabaena sp. PCC 7120 CPB4337. The interactions were quantified by means of the combination index (CI)-isobologram method. The binary mixtures of wastewater with SiO2, SiO2-NH2 and TiO2 displayed antagonism for the lower affected fractions, which corresponded to the lower concentrations. For higher effects and for the Fe3O4 nanoparticles over the whole tested range, the mixtures were additive leading to synergism for the higher affected fractions. No internalization was observed. The results showed that the reduced toxicant bioavailability due to the interaction with nanoparticles is relevant for micropollutants at environmental concentrations. The amount of anthropogenic pollutants retained by metal oxide nanoparticles has significant toxicological effectsFinancial support was provided by FP7-ERA-Net Susfood, 2014/00153/001, the Spanish Ministry of Economy, CTM2013-45775-C2-1-R and CTM2013-45775-C2-2-R and the Dirección General de Universidades e Investigación de la Comunidad de Madrid, Network S2013/MAE-271

Aspectos epidemiológicos de la giardiosis murina en la provincia de Granada

A total of 318 small intestine samples from rats captured in sorne zones of the province of Granada (Spain) have been analized. The parasitation rate was 10'69%, and the highest infection was found in Las Alpujarras (19' 10%). Signifficant differences between males and females were also obtained, the latter showing the highest parasitation. Regarding seasonal distribution, no signifficant differences between seasons were found.Se han analizado 318 muestras intestinales de ratas capturadas en la provincia de Granada, obteniendo un 10'69% de parasitación. De las tres zonas estudiadas (Las Alpujarras, La Costa-Valle de Lecrin y Las Vegas), la primera es la que presenta mayor tasa de parasitación (19'10%), con diferencias significativas del 99% frente a Las Vegas y del 95% frente a La Costa-Valle de Lecrin. Se han encontrado diferencias significativas de parasitación del 95% entre machos y hembras, siendo éstas las más parasitadas. En cuanto a la distribución estacional, si bien el verano y el otoño presentan la mayor y menor tasa, respectivamente, no existe diferencia significativa de parasitación entre ninguna de las estaciones

Estudio de la toxoplasmosis y sarcosporidiosis de ganada bovino de la provincia de Granada (España)

The variations in the content of free amino acids in fruits during ripening is a matter of interest since these compounds are related to their flavour, taste and structure. This study was designed to determine the changes of free amino acids in ripening cherimoya fruits (Annona cherimolia var. Fino de Jete), evaluating the influence of the storage temperature afier harvesting. Methanolic fruit extracts of epicarp and mesocarp were used for quantification of free amino acids which were analyzed by ion-exchange chromatography. Citrulline and proline were detected in relatively high amounts. Glutamate, glutamine, aspartate, asparagine and the non proteinogenic taurine, y-aminobutyric and yaminoadipic acids were found in concentrations that varied between 2-6% of the total free amino acids content. Ripening increased the contents of amino acids, mainly proline,  citrulline and glutamate when cherimoya storage at 20 oC or 80 oC. These increases did not occur when the storage temperature was maintained at 4 oC suggesting that chilling injury markedly affects the synthesis pathway of proline from glutamate.Las variaciones en el contenido de aminoácidos libres en frutos durante la maduración es un tema de interés debido a la relación de estos compuestos con su olor, sabor y estructura. Este estudio se ha diseñado para determinar los cambios en aminoácidos libres durante la maduración de los frutos del chirimoyo (Annona cherimolia varo Fino de Jete), evaluando la influencia de la temperatura de almacenamiento después de la recolección. Extractos metanólicos de epicarpio y mesocarpio del fruto se usaron para la cuantificación de los aminoácidos libres, los cuales fueron analizados por cromatografia de intercambio iónico. Citrulina y prolina se detectaron en cantidades relativamente altas. Glutamato, glutamine, aspartato, asparragina y los no proteinogenéticos taurina, ácido yaminobutíricoy ácido a-aminoadípico fueron encontrados en concentraciones que variaron entre 2-6% del total del contenido de aminoácidos libres. La maduración incrementó el contenido de aminoácidos, sobre todo de prolina, citrulina y glutamato, cuando los chirimoyos se almacenaron a 20 oC o 8 oc. Este incremento no ocurrió cuando la temperatura de almacenamiento se mantuvo a 4 oC, sugiriendo que el daño por frío afecta marcadamente a la vía de síntesis de la prolina a partir de glutamato

Estudio de la toxoplasmosis y sarcosporidiosis en el ganado bovino de la provincia de Granada (España)

Se han examinado, medíante las técnicas de IFI y de dígestión pépsica muscular, un total de 120 muestras procedentes de bovinos sacrificados en el Matadero Municipal de Granada, para el estudio de la toxoplasmosis y sarcosporidiosis bovinas, respectivamente. El porcentaje global de parasitación fue del 85% para Toxoplasma gondii y del 76,6% para Sarcocystis spp. El estudio de la parasitación conjunta por T. gondii y Sarcocystis spp. mostró una independencia matemática entre ambos parasitismos, siendo la independencia ostensiblemente más significativa, tanto global como estacionariamente, en las hembras que en los machos.A total of 120 samples from sacrified in the Granada Municipal Slaughterhouse were tested by pepsic muscular digestion to document sarcosporidiosis and serum were tested by IFAT for antibody to Toxoplasma gondii. The percentage of parasitation was 85"10 for Toxoplasma gondii and 76,6% for Sarcoscystis spp. The study of dual parasitation by T. gondii and Sarcoscystis spp. indicated mathematical independence between the both parasitisms. This independence appeared increasingly more significant in females over males at the as well as in the seasonal leve\