Guía de práctica clínica para la prevención, diagnóstico, tratamiento y rehabilitación de la falla cardiaca en población mayor de 18 años, clasificación B, C y D

La falla cardíaca es un síndrome clínico caracterizado por síntomas y signos típicos de insuficiencia cardíaca, adicional a la evidencia objetiva de una anomalía estructural o funcional del corazón. Guía completa 2016. Guía No. 53Población mayor de 18 añosN/

Hunting Molecules in Complex Matrices with SPME Arrows: A Review

Thirty years since the invention and public disclosure of solid phase microextraction (SPME), the technology continues evolving and inspiring several other green extraction technologies amenable for the collection of small molecules present in complex matrices. In this manuscript, we review the fundamental and operational aspects of a novel SPME geometry that can be used to “hunt” target molecules in complex matrices: the SPME Arrow. In addition, a series of applications in environmental, food, cannabis and forensic analysis are succinctly covered. Finally, special emphasis is placed on novel interfaces to analytical instrumentation, as well as recent developments in coating materials for the SPME Arrow

Rapid determination of tacrolimus and sirolimus in whole human blood by direct coupling of solid-phase microextraction to mass spectrometry via microfluidic open interface

Immunosuppressive drugs are administered to decrease immune system activity (e.g. of patients undergoing solid organ transplant). Concentrations of immunosuppressive drugs (ISDs) in circulating blood must be closely monitored during the period of immunosuppression therapy due to adverse effects that take place when concentration levels fall outside of the very narrow therapeutic concentration range of these drugs. This study presents the rapid determination of four relevant immunosuppressive drugs (tacrolimus, sirolimus, everolimus, and cyclosporine A) in whole human blood by directly coupling solid-phase microextraction to mass spectrometry via the microfluidic open interface (Bio-SPME-MOI-MS/MS). The BioSPME-MOI-MS/MS method offers ≤ 10% imprecision of in-house prepared quality controls over a 10-day period, ≤ 10% imprecision of ClinCal® Recipe calibrators over a three-day period, and single total turnaround time of ∼ 60 min (4.5 min for high throughput). The limits of quantification were determined to be 0.8 ng mL−1 for tacrolimus, 0.7 ng mL−1 sirolimus, 1.0 ng mL−1 for everolimus, and 0.8 ng mL−1 for cyclosporine. The limits of detection were determined to be 0.3 ng mL−1 for tacrolimus, 0.2 ng mL−1 for sirolimus, 0.3 ng mL−1 for everolimus, and 0.3 ng mL−1 for cyclosporine A. The R2 values for all analytes were above 0.9992 with linear dynamic range from 1.0 mL−1 to 50.0 ng mL−1 for tacrolimus, sirolimus, and everolimus while from 2.5 ng mL−1 to 500.0 ng mL−1 for cyclosporine A. To further evaluate the performance of the present method, 95 residual whole blood samples of tacrolimus and sirolimus from patients undergoing immunosuppression therapy were used to compare the Bio-SPME-MOI-MS/MS method against a clinically validated reference method based on chemiluminescent microparticle immunoassay, showing acceptable results. Our results demonstrated that Bio-SPME-MOI-MS/MS can be considered as a suitable alternative to existing methods for the determination of immunosuppressive drugs in whole blood providing faster analysis, better selectivity and sensitivity, and a wider dynamic range than current existing approaches.Fil: Nazdrajic, Emir. University of Waterloo; CanadáFil: Tascon, Marcos. University of Waterloo; Canadá. Universidad Nacional de San Martín. Instituto de Investigación e Ingeniería Ambiental. - Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Parque Centenario. Instituto de Investigación e Ingeniería Ambiental; ArgentinaFil: Rickert, Daniel A.. University of Waterloo; CanadáFil: Gómez Ríos, German A.. University of Waterloo; CanadáFil: Kulasingam, Vathany. University of Toronto; Canadá. University of Toronto; CanadáFil: Pawliszyn, Janusz B.. University of Waterloo; Canad

Assessment Of Solid Phase Microextraction As A Sample Preparation Tool For Metabolomics Analysis Of Brain Tissue By Liquid Chromatography-Mass Spectrometry

This work presents an evaluation of solid-phase microextraction (SPME) SPME in combination with liquid chromatography-high resolution mass spectrometry (LC-HRMS) as an analytical approach for untargeted brain analysis. The study included a characterization of the metabolite coverage provided by C18, mixed-mode (MM, with benzene sulfonic acid and C18 functionalities), and hydrophilic lipophilic balanced (HLB) particles as sorbents in SPME coatings after extraction from cow brain homogenate at static conditions. The effects of desorption solvent, extraction time, and chromatographic modes on the metabolite features detected were investigated. Method precision and absolute matrix effects were also assessed. Among the main findings of this work, it was observed that all three tested coating chemistries were able to provide comparable brain tissue information. HLB provided higher responses for polar metabolites; however, as these fibers were prepared in-house, higher inter-fiber relative standard deviations were also observed. C18 and HLB coatings offered similar responses with respect to lipid-related features, whereas MM and C18 provided the best results in terms of method precision. Our results also showed that the use of methanol is essential for effective desorption of non-polar metabolites. Using a reversed-phase chromatographic method, an average of 800 and 1200 brain metabolite features detected in positive and negative modes, respectively, met inter-fibre RSD values below 30% (n=4) after removal of fibre and solvent artefacts from the associated datasets. For features detected using a lipidomics method, a total of 900 and 1800 features detected using C18 fibers in positive and negative mode, respectively, met the same criteria. In terms of absolute matrix effects, the majority of the model metabolites tested showed values between 80 and 120%, which are within the acceptable range. Overall, the findings of this work lay the foundation for further optimization of parameters for SPME-LC-HRMS methods suitable for in vivo and ex vivo brain (and other tissue) untargeted studies, and support the applicability of this approach for non-destructive tissue metabolomics

Simultaneous Determination of Immunosuppressive Drugs from Whole Blood by CoatedBlade Spray Ionization-Mass Spectrometry

Coated Blade Spray (CBS) ionization was conceived as a fast and simple sampling/sample-preparation and ionization method for qualitative/quantitative mass spectrometry (MS) analysis of drugs of abuse, pharmaceuticals, and other small molecules from urine, blood, and other biofluids. This study describes the use of the CBS for the quantitation of immunosuppressive drugs from 100 µL of blood samples, focusing specifically on the simultaneous quantitation of everolimus, tacrolimus, sirolimus, and cyclosporine-A. These drugs are characterized for having a narrow therapeutic range (e.g. 2-15 ng mL-1, 5-15 ng mL-1, 6-8 ng mL-1, and 100-350 ng mL-1 for tacrolimus (TAC), sirolimus (SIR), everolimus (EVR) and cyclosporine A (CycA), respectively); therefore, continuous monitoring to avoid either subtherapeutic or toxic effect is always required. Our results showed rewarding limits of quantitation (1 ng mL-1 for EVR/SIR/TAC, and 10 ng mL-1 for CycA) as well as good accuracy (• 90 %) and linearity (R2>0.99) over the range evaluated for all the compounds (1-50 ng/mL for EVR/SIR/TAC, and 10-500 ng mL-1 for CycA). The precision of the method was below 15% in all the cases and the bias for three different validation points ranged from 2% to 10%. No matrix effects were observed when evaluating this methodology at different hematocrit levels. By using a high-throughput autosampler, a total analysis time of less than 3 minutes can be attained per sample