DOSY Analysis of Micromolar Analytes: Resolving Dilute Mixtures by SABRE Hyperpolarization

Abstract

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Advancing homogeneous catalysis for parahydrogen-derived hyperpolarisation and its NMR applications

“…50,51 In these examples, peak overlap, even within the hydride region of 1 H NMR spectra, can often become a problem due to the large number of SABRE-amenable analytes in the mixture. It is therefore often advantageous to use 2D NMR methods such as COSY, 188,189 DOSY 190,191 or others 49,51 to provide increased chemical resolution between analytes.…”

Single‐Scan 13C Diffusion‐Ordered NMR Spectroscopy of DNP‐Hyperpolarised Substrates

“…Importantly,s ystematic errors do not prevent the separation of componentsi namixture, or the characterisation of interactions,p rovided that suitable calibrationp rocedures are used. Other hyperpolarisation methods, such as SABRE that has recently been used for multi-scan DOSY analyses, [24] should also be compatiblew ith single-scan acquisitions. [22] D-DNP provides signal enhancements of several orders of magnitude for high-resolution solution-state NMR.…”

“…[23] The actuall imit of detection will also depend on other factors such as sample dilution,a nd the removal or conservation of polarisation agents. Other hyperpolarisation methods, such as SABRE that has recently been used for multi-scan DOSY analyses, [24] should also be compatiblew ith single-scan acquisitions.…”

Membranas de poli (óxido de etileno) e trombina eletrofiadas para reparo de lesões teciduai

“…O experimento de difusão, ou DOSY (Diffusion Ordered Spectroscopy), é uma técnica de espectroscopia de RMN que resolve ressonâncias de acordo com os coeficientes de difusão dos analitos. Destaca-se por fornecer as informações de uma maneira facilmente analisada, possibilitando uma visão global dos tamanhos de partículas em uma amostra e a detecção de impurezas, ou seja, é capaz de determinar componentes de misturas complexas e de baixa molaridade, reduzindo assim os requisitos de concentração em pelo menos 100 vezes (REILE et al, 2017). Sendo assim, a análise RMN -DOSY foi realizada para identificar a presença de trombina e a interação entre as cadeias de PEO/trombina nas membranas, identificando a difusividade do conjunto PEO/Trombina em água e traçando um comparativo com a difusividade do polímero isolado.…”

“…A espectroscopia de ressonância magnética nuclear foi usada para identificar a presença de trombina nas nanofibras PEO/trombina, cujos espectros de RMN-1 H são mostrados na figura 21 A-B. A técnica possui como vantagem conseguir captar concentrações mínimas em misturas de substâncias (REILE et al, 2017), o que nem sempre é possível em outras técnicas como FTIR, por exemplo. O espectro de PEO/Trombina mostrou sinais de ambos os componentes…”