Química Analítica : materiales docentes : grado de Ingeniería Química, 2º curso

El capítulo 1 está dedicado al proceso analítico y a las propiedades analíticas que afectan a la calidad del resultado y del procedimiento de análisis químico. El capítulo 2 describe el muestreo y diferentes procesos de preparación de muestra. El capítulo 3 trata de los diferentes métodos volumétricos de análisis, incluyendo las valoraciones ácido-base, de formación de complejos, en medio heterogéneo y de oxidaciónreducción. Los tres capítulos siguientes están relacionados con los métodos espectroscópicos. El capítulo 4 es un tema de introducción a los métodos instrumentales en el que se describen los métodos de calibración, las fuentes de ruido y las características, especificaciones y clasificación de los analizadores de procesos y incluyendo el analizador continuo de flujo no segmentado. El capítulo 5 describe los métodos espectroscópicos en UV-Visible e IR, sus principios básicos, IV Prólogo componentes, función y requerimientos. El capítulo 6 está dedicado a los métodos espectroscópicos de análisis molecular, fundamento, aplicaciones y manejo de instrumentos. En el capítulo 7 se describe las características generales y aplicaciones de las técnicas de espectroscopía atómica o elemental. El capítulo 8 se dedica a las generalidades de la cromatografía, incluyendo el fundamento y aplicaciones de la cromatografía de gases y la detección por espectrometría de masas. El capítulo 9 describe los aspectos básicos e instrumentación de la cromatografía de líquidos de alta resolución y su acoplamiento a espectrometría de masas. Finalmente, en el capítulo 10 se describe el fundamento clasificación y aplicaciones de los sensores electroanalíticos.En el marco del Espacio Europeo de Educación Superior (EEES), cobra especial relevancia el impacto de las Tecnologías de la Información y la Comunicación (TICs) con posibilidades tanto para la elaboración del conocimento como para su adquisición y transmisión, mediante métodos pedagógicos más innovadores, adcesibles e interactivos que se adapten a los diferentes tipos de estudiantes. El acceso a las redes de la información dotan al docente y al alumnado de poderosas herramientas que abren un gran abanico de posibilidades metodológicas. Siguiendo esta línea, el ámbito de aplicación de este material docente corresponde a la materia de enseñanza-aprendizaje de “Química Analítica” de segundo curso (primer semestre) de la titulación de Grado en Ingeniería Química impartida en la Escuela Técnica Superior de Ingeniería (ETSE) de la Universidad de Santiago de Compostela

Development of a QuEChERS method for simultaneous analysis of 3-Monochloropropane-1,2-diol monoesters and Glycidyl esters in edible oils and margarine by LC-APCI-MS/MS

A simple, fast and effective direct method based on HPLC-APCI-QqQ-MS/MS has been developed to simultaneously determine four 3-monochloropropane-1,2-diol monoesters (3-MCPDE) esterified with palmitic, linoleic, stearic, and oleic acid, and two glycidyl esters (GE) with palmitic and oleic acid in margarine and olive oil using a QuEChERS approach. Factors affecting the efficiency of the extraction process were assessed, including type and amount of salt, extraction solvent, test portion amount, and clean-up sorbent. The analytical method was validated according to Food and Drug Administration (FDA) guidelines using matrix-matched calibration with internal standards and showed good results in terms of linearity (r2 > 0.9992), accuracy (80<Recovery<120%), and precision (RSD<15%). The method was successfully applied for the first time to 11 margarine samples for simultaneous analysis of 3-MCPDE and GEThis work was supported by the Spanish Ministry of Science, Innovation, and Universities (Project RTI2018‐096450‐B‐I00) and FEDER fundsS

Determination of synthetic opioids in oral fluid samples using fabric phase sorptive extraction and gas chromatography-mass spectrometry

New psychoactive substances (NPS) continue to emerge in the drug market every year, becoming a global threat to public health and safety. These compounds are mostly synthetic cannabinoids and designer cathinones. However, synthetic opioids have appeared on the recreational drug markets in recent years, particularly fentanyl and its derivatives (“fentanyls”). Fentanyl and its analogs are related to harmful intoxications and an increase in opioid-related mortality in many countries, such as in the United States and Europe in the last years. Taking the drug related global crisis into consideration, this work developed and validated an effective and sensitive method based on fabric phase sorptive extraction (FPSE) followed by gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of 11 fentanyl analogs in oral fluid samples. The extraction was carried out using a sol-gel Carbowax 20 M sorbent immobilized on 100% cellulose fabric substrate and using ethyl acetate as the desorption solvent. The limits of detection (LODs) and quantification (LOQs) ranged from 1 to 15 ng mL−1 and 5 to 50 ng mL−1, respectively. Intra-day and inter-day precision were found within 8.2% and 8.6%, respectively, while accuracy ranged from -5.5 to 9.1%, in accordance with the established criteria. The absolute recovery values were in the range of 94.5%–109.1%. The validated method demonstrated its great potential to detect and quantify fentanyl analogs in possible forensic work and off-site analysis in road traffic casesThis work was supported by the Spanish Ministry of Science, Innovation, and Universities (Project RTI2018‐096450‐B‐I00) and FEDER fundsS

Treatment with tocilizumab or corticosteroids for COVID-19 patients with hyperinflammatory state: a multicentre cohort study (SAM-COVID-19)

Objectives: The objective of this study was to estimate the association between tocilizumab or corticosteroids and the risk of intubation or death in patients with coronavirus disease 19 (COVID-19) with a hyperinflammatory state according to clinical and laboratory parameters. Methods: A cohort study was performed in 60 Spanish hospitals including 778 patients with COVID-19 and clinical and laboratory data indicative of a hyperinflammatory state. Treatment was mainly with tocilizumab, an intermediate-high dose of corticosteroids (IHDC), a pulse dose of corticosteroids (PDC), combination therapy, or no treatment. Primary outcome was intubation or death; follow-up was 21 days. Propensity score-adjusted estimations using Cox regression (logistic regression if needed) were calculated. Propensity scores were used as confounders, matching variables and for the inverse probability of treatment weights (IPTWs). Results: In all, 88, 117, 78 and 151 patients treated with tocilizumab, IHDC, PDC, and combination therapy, respectively, were compared with 344 untreated patients. The primary endpoint occurred in 10 (11.4%), 27 (23.1%), 12 (15.4%), 40 (25.6%) and 69 (21.1%), respectively. The IPTW-based hazard ratios (odds ratio for combination therapy) for the primary endpoint were 0.32 (95%CI 0.22-0.47; p < 0.001) for tocilizumab, 0.82 (0.71-1.30; p 0.82) for IHDC, 0.61 (0.43-0.86; p 0.006) for PDC, and 1.17 (0.86-1.58; p 0.30) for combination therapy. Other applications of the propensity score provided similar results, but were not significant for PDC. Tocilizumab was also associated with lower hazard of death alone in IPTW analysis (0.07; 0.02-0.17; p < 0.001). Conclusions: Tocilizumab might be useful in COVID-19 patients with a hyperinflammatory state and should be prioritized for randomized trials in this situatio

Post-intervention Status in Patients With Refractory Myasthenia Gravis Treated With Eculizumab During REGAIN and Its Open-Label Extension

OBJECTIVE: To evaluate whether eculizumab helps patients with anti-acetylcholine receptor-positive (AChR+) refractory generalized myasthenia gravis (gMG) achieve the Myasthenia Gravis Foundation of America (MGFA) post-intervention status of minimal manifestations (MM), we assessed patients' status throughout REGAIN (Safety and Efficacy of Eculizumab in AChR+ Refractory Generalized Myasthenia Gravis) and its open-label extension. METHODS: Patients who completed the REGAIN randomized controlled trial and continued into the open-label extension were included in this tertiary endpoint analysis. Patients were assessed for the MGFA post-intervention status of improved, unchanged, worse, MM, and pharmacologic remission at defined time points during REGAIN and through week 130 of the open-label study. RESULTS: A total of 117 patients completed REGAIN and continued into the open-label study (eculizumab/eculizumab: 56; placebo/eculizumab: 61). At week 26 of REGAIN, more eculizumab-treated patients than placebo-treated patients achieved a status of improved (60.7% vs 41.7%) or MM (25.0% vs 13.3%; common OR: 2.3; 95% CI: 1.1-4.5). After 130 weeks of eculizumab treatment, 88.0% of patients achieved improved status and 57.3% of patients achieved MM status. The safety profile of eculizumab was consistent with its known profile and no new safety signals were detected. CONCLUSION: Eculizumab led to rapid and sustained achievement of MM in patients with AChR+ refractory gMG. These findings support the use of eculizumab in this previously difficult-to-treat patient population. CLINICALTRIALSGOV IDENTIFIER: REGAIN, NCT01997229; REGAIN open-label extension, NCT02301624. CLASSIFICATION OF EVIDENCE: This study provides Class II evidence that, after 26 weeks of eculizumab treatment, 25.0% of adults with AChR+ refractory gMG achieved MM, compared with 13.3% who received placebo

Minimal Symptom Expression' in Patients With Acetylcholine Receptor Antibody-Positive Refractory Generalized Myasthenia Gravis Treated With Eculizumab

The efficacy and tolerability of eculizumab were assessed in REGAIN, a 26-week, phase 3, randomized, double-blind, placebo-controlled study in anti-acetylcholine receptor antibody-positive (AChR+) refractory generalized myasthenia gravis (gMG), and its open-label extension

Search for dark matter produced in association with bottom or top quarks in √s = 13 TeV pp collisions with the ATLAS detector

A search for weakly interacting massive particle dark matter produced in association with bottom or top quarks is presented. Final states containing third-generation quarks and miss- ing transverse momentum are considered. The analysis uses 36.1 fb−1 of proton–proton collision data recorded by the ATLAS experiment at √s = 13 TeV in 2015 and 2016. No significant excess of events above the estimated backgrounds is observed. The results are in- terpreted in the framework of simplified models of spin-0 dark-matter mediators. For colour- neutral spin-0 mediators produced in association with top quarks and decaying into a pair of dark-matter particles, mediator masses below 50 GeV are excluded assuming a dark-matter candidate mass of 1 GeV and unitary couplings. For scalar and pseudoscalar mediators produced in association with bottom quarks, the search sets limits on the production cross- section of 300 times the predicted rate for mediators with masses between 10 and 50 GeV and assuming a dark-matter mass of 1 GeV and unitary coupling. Constraints on colour- charged scalar simplified models are also presented. Assuming a dark-matter particle mass of 35 GeV, mediator particles with mass below 1.1 TeV are excluded for couplings yielding a dark-matter relic density consistent with measurements

Identification of genetic variants associated with Huntington's disease progression: a genome-wide association study

Background Huntington's disease is caused by a CAG repeat expansion in the huntingtin gene, HTT. Age at onset has been used as a quantitative phenotype in genetic analysis looking for Huntington's disease modifiers, but is hard to define and not always available. Therefore, we aimed to generate a novel measure of disease progression and to identify genetic markers associated with this progression measure. Methods We generated a progression score on the basis of principal component analysis of prospectively acquired longitudinal changes in motor, cognitive, and imaging measures in the 218 indivduals in the TRACK-HD cohort of Huntington's disease gene mutation carriers (data collected 2008–11). We generated a parallel progression score using data from 1773 previously genotyped participants from the European Huntington's Disease Network REGISTRY study of Huntington's disease mutation carriers (data collected 2003–13). We did a genome-wide association analyses in terms of progression for 216 TRACK-HD participants and 1773 REGISTRY participants, then a meta-analysis of these results was undertaken. Findings Longitudinal motor, cognitive, and imaging scores were correlated with each other in TRACK-HD participants, justifying use of a single, cross-domain measure of disease progression in both studies. The TRACK-HD and REGISTRY progression measures were correlated with each other (r=0·674), and with age at onset (TRACK-HD, r=0·315; REGISTRY, r=0·234). The meta-analysis of progression in TRACK-HD and REGISTRY gave a genome-wide significant signal (p=1·12 × 10−10) on chromosome 5 spanning three genes: MSH3, DHFR, and MTRNR2L2. The genes in this locus were associated with progression in TRACK-HD (MSH3 p=2·94 × 10−8 DHFR p=8·37 × 10−7 MTRNR2L2 p=2·15 × 10−9) and to a lesser extent in REGISTRY (MSH3 p=9·36 × 10−4 DHFR p=8·45 × 10−4 MTRNR2L2 p=1·20 × 10−3). The lead single nucleotide polymorphism (SNP) in TRACK-HD (rs557874766) was genome-wide significant in the meta-analysis (p=1·58 × 10−8), and encodes an aminoacid change (Pro67Ala) in MSH3. In TRACK-HD, each copy of the minor allele at this SNP was associated with a 0·4 units per year (95% CI 0·16–0·66) reduction in the rate of change of the Unified Huntington's Disease Rating Scale (UHDRS) Total Motor Score, and a reduction of 0·12 units per year (95% CI 0·06–0·18) in the rate of change of UHDRS Total Functional Capacity score. These associations remained significant after adjusting for age of onset. Interpretation The multidomain progression measure in TRACK-HD was associated with a functional variant that was genome-wide significant in our meta-analysis. The association in only 216 participants implies that the progression measure is a sensitive reflection of disease burden, that the effect size at this locus is large, or both. Knockout of Msh3 reduces somatic expansion in Huntington's disease mouse models, suggesting this mechanism as an area for future therapeutic investigation

Prevalence, associated factors and outcomes of pressure injuries in adult intensive care unit patients: the DecubICUs study

Funder: European Society of Intensive Care Medicine; doi: http://dx.doi.org/10.13039/501100013347Funder: Flemish Society for Critical Care NursesAbstract: Purpose: Intensive care unit (ICU) patients are particularly susceptible to developing pressure injuries. Epidemiologic data is however unavailable. We aimed to provide an international picture of the extent of pressure injuries and factors associated with ICU-acquired pressure injuries in adult ICU patients. Methods: International 1-day point-prevalence study; follow-up for outcome assessment until hospital discharge (maximum 12 weeks). Factors associated with ICU-acquired pressure injury and hospital mortality were assessed by generalised linear mixed-effects regression analysis. Results: Data from 13,254 patients in 1117 ICUs (90 countries) revealed 6747 pressure injuries; 3997 (59.2%) were ICU-acquired. Overall prevalence was 26.6% (95% confidence interval [CI] 25.9–27.3). ICU-acquired prevalence was 16.2% (95% CI 15.6–16.8). Sacrum (37%) and heels (19.5%) were most affected. Factors independently associated with ICU-acquired pressure injuries were older age, male sex, being underweight, emergency surgery, higher Simplified Acute Physiology Score II, Braden score 3 days, comorbidities (chronic obstructive pulmonary disease, immunodeficiency), organ support (renal replacement, mechanical ventilation on ICU admission), and being in a low or lower-middle income-economy. Gradually increasing associations with mortality were identified for increasing severity of pressure injury: stage I (odds ratio [OR] 1.5; 95% CI 1.2–1.8), stage II (OR 1.6; 95% CI 1.4–1.9), and stage III or worse (OR 2.8; 95% CI 2.3–3.3). Conclusion: Pressure injuries are common in adult ICU patients. ICU-acquired pressure injuries are associated with mainly intrinsic factors and mortality. Optimal care standards, increased awareness, appropriate resource allocation, and further research into optimal prevention are pivotal to tackle this important patient safety threat