RESUMO
Quantitative nuclear magnetic resonance (qNMR) is a well-established technique in quantitative analysis. We presented a validated 1 H-qNMR method for assay of octreotide acetate, a kind of cyclic octopeptide. Deuterium oxide was used to remove the undesired exchangeable peaks, which was referred to as proton exchange, in order to make the quantitative signals isolated in the crowded spectrum of the peptide and ensure precise quantitative analysis. Gemcitabine hydrochloride was chosen as the suitable internal standard. Experimental conditions, including relaxation delay time, the numbers of scans, and pulse angle, were optimized first. Then method validation was carried out in terms of selectivity, stability, linearity, precision, and robustness. The assay result was compared with that by means of high performance liquid chromatography, which is provided by Chinese Pharmacopoeia. The statistical F test, Student's t test, and nonparametric test at 95% confidence level indicate that there was no significant difference between these two methods. qNMR is a simple and accurate quantitative tool with no need for specific corresponding reference standards. It has the potential of the quantitative analysis of other peptide drugs and standardization of the corresponding reference standards.
Assuntos
Octreotida/química , Calibragem , Óxido de Deutério/química , Espectroscopia de Prótons por Ressonância Magnética/normas , Padrões de ReferênciaRESUMO
We report a facile and generic method for the synthesis of hollow mesoporous silica nanoreactors (HMSNs) with small-sized metal oxide nanoparticles (NPs) inside their cavities. They were made by deposition of silica onto metal-containing charge-driven polymer micelles and subsequent calcination. The micelles consist of 1)â negatively charged supramolecular polyelectrolyte chains of bis-ligand-bound metal ions, and 2)â water-soluble, neutral/positive diblock copolymers. Owing to the facile coordination between transition-metal ion and the employed bidentate ligand, a series of HMSNs with <2â nm Mx Oy NPs inside cavities (M=Mn, Co, Ni, Cu, or Zn) were obtained by simply varying the metal ions inside the micelles. The developed method circumvents the pre- and post-synthesis of metal oxide NPs; after calcination, hollow mesoporous nanostructures containing small-sized metal oxide NPs inside their cavities are directly obtained. The Cox Oy -functionalized HMSNs catalyze the degradation of various dyes with H2 O2 .
RESUMO
The precise identification of arrhythmia is critical in electrocardiogram (ECG) research. Many automatic classification methods have been suggested so far. However, efficient and accurate classification is still a challenge due to the limited feature extraction and model generalization ability. We integrate attention mechanism and residual skip connection into the U-Net (RA-UNET); besides, a skip connection between the RA-UNET and a residual block is executed as a residual attention convolutional neural network (RA-CNN) for accurate classification. The model was evaluated using the MIT-BIH arrhythmia database and achieved an accuracy of 98.5% and F 1 scores for the classes S and V of 82.8% and 91.7%, respectively, which is far superior to other approaches.
Assuntos
Algoritmos , Eletrocardiografia , Arritmias Cardíacas/diagnóstico , Bases de Dados Factuais , Progressão da Doença , Humanos , Redes Neurais de Computação , Processamento de Sinais Assistido por ComputadorRESUMO
Worm-like nanowires are among the most active nanomaterials. In this study, we report the synthesis of dibenzylamine (DBA) motifs from reductive amination of either aldehydes or nitriles catalyzed by entirely new worm-like PtMo nanowires (PtMo WNWs). Under the assistance of H2 gas, PtMo WNWs can be prepared in a facile manner, following which, their structure and composition are characterized by TEM, XRD, XPS, etc. Upon careful optimization of reaction parameters, the as-prepared PtMo WNWs work effectively in the activation of dihydrogen molecules, and both aldehydes and nitriles can be used as starting materials to fabricate DBAs under mild and green conditions. The reaction kinetics has been investigated, which reveals that the PtMo WNWs show superior activity in the conversion of imines into amines. This study provides a practical advancement in the preparation of amines. Moreover, the protocol reported herein is feasible for the synthesis of worm-like nanostructures with designed composition for various catalytic applications.