RESUMO
PURPOSE: A novel dissolution dynamic nuclear polarization (dDNP) polarizer platform is presented. The polarizer meets a number of key requirements for in vitro, preclinical, and clinical applications. METHOD: It uses no liquid cryogens, operates in continuous mode, accommodates a wide range of sample sizes up to and including those required for human studies, and is fully automated. RESULTS: It offers a wide operational window both in terms of magnetic field, up to 10.1 T, and temperature, from room temperature down to 1.3 K. The polarizer delivers a 13 C liquid state polarization for [1-13 C]pyruvate of 70%. The build-up time constant in the solid state is approximately 1200 s (20 minutes), allowing a sample throughput of at least one sample per hour including sample loading and dissolution. CONCLUSION: We confirm the previously reported strong field dependence in the range 3.35 to 6.7 T, but see no further increase in polarization when increasing the magnetic field strength to 10.1 T for [1-13 C]pyruvate and trityl. Using a custom dry magnet, cold head and recondensing, closed-cycle cooling system, combined with a modular DNP probe, and automation and fluid handling systems, we have designed a unique dDNP system with unrivalled flexibility and performance.
Assuntos
Espectroscopia de Ressonância Magnética Nuclear de Carbono-13/instrumentação , Campos Magnéticos , Espectroscopia de Ressonância Magnética/instrumentação , Espectroscopia de Ressonância Magnética/métodos , Algoritmos , Espectroscopia de Ressonância Magnética Nuclear de Carbono-13/métodos , Desenho de Equipamento , Hélio , Temperatura Alta , Magnetismo , Reconhecimento Automatizado de Padrão , Ácido Pirúvico/química , Software , Temperatura , Fatores de TempoRESUMO
The desire for higher magnetic resonance sensitivity has led to the development of multiple home-built and commercial dissolution dynamic nuclear polarization polarizers. The emergence of polarizers capable of variable magnetic field strengths desires a versatile standalone spectrometer and NMR circuit to fulfill detection needs at different frequencies. We present a benchtop NMR spectrometer with a duplexer capable of serving high-field solid and liquid state NMR applications up to 450â¯MHz. A detailed view of the employed probe is discussed. Tuning and matching schemes are investigated yielding and experimentally verifying closed-form equations to estimate the nutation frequency for a remotely tuned and matched sample coil.