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增强固态 NMR 的灵敏度

作为市场领导品牌,布鲁克引入了世界第一款市售固态动态核极化增强型 NMR 系统 (DNP-NMR)

布鲁克的 263、395 和 527 GHz DNP-NMR 光谱仪是世界上第一批市售固态动态核极化 (DNP-NMR) 系统。所有 DNP-NMR 质谱仪对生物分子研究、材料科学和制药领域的现有新型应用具有非常高的灵敏度,可使扩展后的固态 NMR 实验得以进行。布鲁克 DNP 质谱仪在全球安装的超过 25 种的系统中均有性能证明记录。

通过添加极化剂或利用所试样品的本体自由基来制备 DNP 样品。进行实验时使用约 100 K 的低温,伴随持续的微波辐照,受益于新型低温 MAS 探头,使得原位样品极化直接在 NMR 场得以实现。

由于微波辐射,极化状态从不成对电子自旋转变为核自旋,信号从 20 倍增强至 200 倍。独特的高功率振动陀螺仪系统,以 263 GHz、395 GHz、527 GHz 发射微波,稳定、安全、易操作,可进行长期 DNP 实验,不受时间限制。

Dnp boltzmann polarization
  • 高磁场 DNP 增强型固体 NMR 实验的完整解决方案
  • 极化增强使固态 NMR 产生了高达 200 倍的灵敏度增益
  • 独特的高功率微波源
  • 由软件控制的易用高功率振动陀螺仪
  • 微波传输线确保了样品的最佳光束传播
  • 含内置波导及冷旋压供气的低温 MAS 探头技术
  • AVANCE™ III HD 400、600、800 大口径 NMR 系统,含扫描线圈

超越不可能

与 Robert Griffin 教授一起研究动态核极化 (DNP) 的开发与商业化。

[Bitte nach "Chinese (Simplified)" übersetzen:] Moving beyond the horizon of possibility

[Bitte nach "Chinese (Simplified)" übersetzen:] Development and Commercialization of Dynamic Nuclear Polarization (DNP) with Professor Robert Griffin.

Gyrotron Microwave Source

The gyrotron includes a sealed custom-designed gyrotron tube, superconducting magnet, and control system, all designed to provide high stability, reliability, and ease of operation. Beam propagation to the sample is ensured by high microwave beam quality and corrugated waveguide. The sample is polarized in-situ in a low-temperature NMR MAS probe.

1H NMR FrequencyWB NMR MagnetGyrotron FrequencyGyrotron Magnet
400 MHz400/89 Ascend DNP 263 GHz 4.8 T cryogen-free
600 MHz 600/89 Ascend DNP 395 GHz7.2 T cryogen-free
800 MHz 800/89 USP RS 527 GHz 9.7 T cryogen-free

263 GHz Klystron Microwave Source

The 263 GHz klystron is a continuous-wave microwave source designed and manufactured for extended DNP NMR at 400 MHz 1H frequency and 100 K sample temperature. The klystron provides a DNP option with lower purchase price, operating costs, footprint, and facility requirements compared to the gyrotron product line while retaining high DNP sensitivity and stability. At 5 W output power, it reaches 90-100% DNP efficiency on biological samples and small molecules in frozen solution while dense material samples perform at > 80% compared to the 263 GHz gyrotron.

The system assembly consists of: (1) extended interaction klystron oscillator (EIK), (2) a control system with graphical user interface, safety interlocks, power supply and cooling network, and (3) a low-loss microwave transmission line. It is compatible with a 400 WB Ascend DNP solid-state NMR spectrometer and Bruker low-temperature MAS (LTMAS) probes.

LT MAS Probe

  • Low sample temperature (~ 100 K)
  • Cold sample coil and RF circuit
  • 3.2 mm MAS rotor (15 kHz max at 100 K)
  • WB triple or double resonance probe (HCN, HXY, or HX NMR circuits))
  • Insert/eject of cold samples
  • Dry low-temperature nitrogen gas supply
  • 3 cold gas lines: bearing, drive and VT
  • Automatic refill of liquid nitrogen supply
  • Waveguide for microwave irradiation
  • Long term operation (days, weeks)
Image technical dnp enc2016
263 GHz Klystron

1.3 and 1.9 mm DNP MAS Probe

DNP experiments are performed at low temperature (100 K) for efficient transfer of polarization from electron spins to nuclear spins. Until recently, the spinning frequency at 100 K was limited to 15 kHz with a 3.2 mm rotor. With the introduction of the Bruker 1.3 and 1.9 mm low-temperature MAS (LTMAS) probe, DNP experiments can now be performed at up to 40 kHz (1.3) and 24 kHz (1.9) MAS MAS frequency for enhanced spectral resolution. The fast MAS probes include pneumatic insert/eject capability at ambient and cold temperature. The ability to change samples while the probe remains cold is critical for optimal use of experiment time. The probe is available with HCN, HXY, or HX NMR circuits.

Control Systems

  • User interface
  • Controls and regulation
  • Temperatures, voltages, water cooling, gyrotron magnet

Sample Preparation and DNP-Enhanced CPMAS of 13C-Proline

The DNP samples are prepared by adding a polarizing agent (such as e.g. TOTAPOL biradical) to a shared solvent or alternatively by utilizing a native radical on the sample of interest. The samples are measured under MAS while at low temperatures, typically 100–120 K. Unmodified NMR experiments are performed while benefitting from continuously DNP-enhanced signal intensity through CW microwave irradiation.

DNP-Enhanced CPMAS

Improved sensitivity from DNP allows the characterization of expansin protein binding to plant cell walls

DNP experiments allow rapid detection of ~1% U-13C,15N expansin mixed with plant cell walls. A REDOR filter selects only signals from the expansin 13C signals and spin diffusion mixing following the REDOR filter reveals correlations between expansin and the cell-wall polysaccharides. Comparison of the wild-type protein with two mutants indicate that site-specific cellulose binding is correlated with strong wall-loosening activity.

DNP fig3 improved

DNP-enhanced NMR in biological solids

A wide range of biological samples have been successfully enhanced on the Bruker DNP-NMR spectrometer including small peptides, soluble proteins, membrane proteins, and large biological complexes.

DNP-enhanced NMR in biological solids

Material Science

DNP NMR allows the characterization, at the molecular level, of hybrid organic silica material. These materials are key compounds for applications in catalysis, drug delivery, separation and purification devices.

DNP in material science
DNP experiments on natural abundance Mat-PrIm

DNP with Fast MAS: Rapid Structural Characterization

25 kHz MAS improves the resolution of DNP spectra, enables long-range inter-residue polarization transfers, and is helpful for extending assignments. DNP experiments were performed on Pf1 bacteriophage with non-uniform sampling (NUS) for rapid acquisition of multidimensional experiments.

DNP with Fast MAS

LabScape

服务和生命周期支持

从初期的产品、技术咨询到仪器的评估、安装和使用,在整个采购周期中我们为客户提供专业详尽的帮助,这一理念和承诺现在已经成为了 LabScape 服务的核心观念

 

LabScape 维修保养服务协议、现场应需服务和实验室改进计划都旨在为现代化的实验室提供维护和服务的新方案。

 

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