Arsenosugar standards extracted from algae: Isolation, characterization and use for identification and quantification purposes

Sulfate (SO4-sug) and sulfonate (SO3-sug) arsenosugar standard solutions were obtained using preparative liquid chromatography. Several commercial algae samples were characterized (total contents and speciation) to select the most appropriate in relation to their arsenosugar contents. Water extracts from the selected sample (Fucus vesiculosus) were fractionated using a Hamilton PRP-X100 preparative column, and the presence of arsenic species in the isolated fractions was ascertained by IC-ICP-MS. Two of the fractions successfully presented only one arsenic species corresponding to sulfate and sulfonate arsenosugars at suitable concentrations. To unequivocally confirm the presence of both compounds, high-resolution mass spectrometry (ESITOF/ MS) was used and the exact mass determined with errors lower than 0.5 ppm. The standard solutions obtained were successfully used to identify and quantify SO4-sug and SO3-sug in several edible algae samples purchased in local market. Total arsenic content for analysed samples ranged from 34 to 57 mg·kg-1, concentration values found for SO3-sug ranged from 5 to 36 mg As·kg-1 and SO4-sug was only found in fucus with a concentration of 9,3 mg As·kg-1

Untargeted Comprehensive Two-Dimensional Liquid Chromatography Coupled with High-Resolution Mass Spectrometry Analysis of Rice Metabolome Using Multivariate Curve Resolution

In this work, a new strategy for the chemometric analysis of two-dimensional liquid chromatography-high-resolution mass spectrometry (LC × LC-HRMS) data is proposed. This approach consists of a preliminary compression step along the mass spectrometry (MS) spectral dimension based on the selection of the regions of interest (ROI), followed by a further data compression along the chromatographic dimension by wavelet transforms. In a secondary step, the multivariate curve resolution alternating least squares (MCR-ALS) method is applied to previously compressed data sets obtained in the simultaneous analysis of multiple LC × LC-HRMS chromatographic runs from multiple samples. The feasibility of the proposed approach is demonstrated by its application to a large experimental data set obtained in the untargeted LC × LC-HRMS study of the effects of different environmental conditions (watering and harvesting time) on the metabolism of multiple rice samples. An untargeted chromatographic setup coupling two different liquid chromatography (LC) columns [hydrophilic interaction liquid chromatography (HILIC) and reversed-phase liquid chromatography (RPLC)] together with an HRMS detector was developed and applied to analyze the metabolites extracted from rice samples at the different experimental conditions. In the case of the metabolomics study taken as example in this work, a total number of 154 metabolites from 15 different families were properly resolved after the application of MCR-ALS. A total of 139 of these metabolites could be identified by their HRMS spectra. Statistical analysis of their concentration changes showed that both watering and harvest time experimental factors had significant effects on rice metabolism. The biochemical insight of the effects of watering and harvesting experimental factors on the changes in concentration of these detected metabolites in the investigated rice samples is attempted. © 2017 American Chemical Society.The research leading to these results has received funding from the European Research Council under the European Union's Seventh Framework Programme (FP/2007-2013)/ERC Grant Agreement No. 320737. The authors would like to thank CRAG for kindly supplying Japanese rice seeds. CTQ2015- 66254-C2-1-P project from MINCO (Spain) is also acknowledged.Peer reviewe

Analgesia con morfina intratecal en cirugía de las deformidades raquídeas

Introducción: la efectividad y seguridad en el control de la analgesia postoperatoria forman una combinación difícil de alcanzar, especialmente en la población pediátrica. En nuestro estudio pretendemos evaluar la eficacia de la morfina administrada de forma intratecal a pequeñas dosis, la calidad de la analgesia y la aparición de efectos secundarios en pacientes adolescentes, sometidos a cirugía correctora de las deformidades raquídeas. Material y método: estudiamos un total de 36 pacientes (11 V /25 M) que fueron intervenidos de cifoescoliosis desde Febrero hasta Diciembre de 1994. La etiología de la deformidad raquídea era en 26 pacientes idiopática y en 10 pacientes secundaria a una enfermedad neuromuscular. A todos ellos se les practicó el mismo examen preoperatorio según protocolo del Servicio y la misma técnica anestésica. Al finalizar la artrodesis vertebral, bajo visión directa el cirujano realizaba la punción en el espacio vertebral L4/L5, L3/L4 con una aguja n2 25 G de punta de lápiz y, administraba la morfina preparada por el Servicio de Farmacia con solución salina apirógena a concentración de 0,1 mg.ml·1 a dosis de 0,01 mg.kg·1, hasta dosis máximas de 0,5 mg en total. Valorábamos, la hora de aparición del dolor, la necesidad de módicos u otros analgésicos parenterales para el control del dolor, la aparición de electos secundarios y si se precisó de naloxona, y también, recogíamos el grado de confort del paciente mediante una modificación de la escala analógica visual (V AS). Resultados: la edad media de los pacientes fue de 15,36 años (11-19). el peso de 54,58 kg (35-78) y la talla 162 cm (142- 187). El tiempo medio de analgesia mórfico dependiente fue de 24,25 horas (1,30-64). Un total de 23 pacientes (63,8%) no precisaron ningún tipo de analgésicos durante su estancia en la sala de reanimación, en 12 pacientes (33,3%) se administraron analgésicos de tipo AINE y sólo en 1 paciente (2,77%) hubo necesidad de administrar mórlicos parenterales para el control del dolor. En cuanto a los electos secundarios, no se registró ningún caso de depresión respiratoria, somnolencia, cefalea, ni prurito. Aparecieron vómitos en 13 pacientes (36, 1 %) y náuseas en 4 ( 11 , 1 %) que no precisaron de la administración de naloxona para su control. La analgesia fue calificada como excelente en el 69,2% de los pacientes idiopáticos y en el 70% en el caso de los secundarios. Conclusiones: la morfina intratecal a dosis aproximadas de 0,01 mg.kg·1 para el control del dolor postoperatorio en la cirugía de la escoliosis es electiva, segura y confortable. Evitando la administración de mórlicos por vía parenteral, los pacientes son capaces de realizar una fisioterapia respiratoria activa, consiguiendo así una recuperación más temprana