Although the nuclear magnetic resonance (NMR) application is very extensive, but its inherent challenge is limited sensitivity.A don't need to change the sample can improve the sensitivity of the method is rf coil and preamplifier cryogenic cooling electronic components.
By the rf coil, network and a preamplifier thermal noise level lower signal-to-noise ratio increase 3 times, and at the same time keep sample in its original elements and the natural line width.This report comes from the first 600 MHz 3.2 mm HCN three resonance CPMAS CryoProbe the results obtained.
Hole probe design for standard magnets, with mature CryoPlatform compatible.Radio frequency (rf) coils and preamplifier electronics cryogenic cooling, compared with the traditional probe, sensitivity to gain more than 3.This is the sample of gain at room temperature.
When using 3.2 mm rotor and MAS3 device, probe the MAS rate of up to 20 kHz.CPMAS CryoProbe probes can be used in cooling state new levelers reduce probe, facilitate safe replacement of the rotor.Automatic tuning and matching increased the probe of the comfortable and safe operation.
BioSolids CryoProbe allowed at physiological temperature research challenging biological systems, and will not change the sample composition.
This feature is very important in the structural biology, because the temperature around the integrity of the protein and is vital for maintaining biological functions are often.
Diluting the samples, such as marker protein or large components in the original environment of small molecules, and the level of natural abundance and low mark sample, benefit from a probe significantly increased the sensitivity of the innovation.
Environment in pharmacology, the probe allows extension NMR toolkit.2 d 13 c13c related experiments can be used in the natural abundance advanced characterization of active pharmaceutical ingredients.Other applications include drug polymorphisms and drug delivery system
Faster data collection
Amyloid fibrils and prions
About 96.7 mg (u - 13 c and 15 n) HET -s (218-289) of prions domain, by the French bordeaux CNRS a. Loquet professor
Due to enhanced sensitivity, spectral record an order of magnitude faster, just need a scan can record spectrogram, and signal to noise ratio and resolution are high.
Faster data collection
Amyloid fibrils and prions
About 96.7 mg (u - 13 c and 15 n) HET -s (218-289) of prions domain, by the French bordeaux CNRS a. Loquet professor
Due to enhanced sensitivity, spectral record an order of magnitude faster, just need a scan can record spectrogram, and signal to noise ratio and resolution are high.
This can save the multidimensional experiment set and get a lot of time.
increaseA dimension
Amyloid fibrils and prions
About 96.7 mg (u - 13 c and 15 n) HET -s (218-289) of prions domain, by the French bordeaux CNRS a. Loquet professor
With the help of BioSolids provide the sensitivity of CryoProbe, scanning frequency can be greatly reduced.Therefore, multidimensional experiment becomes faster.Then, you can take for a period of 2 d experiments run 3 d experiments.In addition, due to the acquisition time is too long and usually does not perform 4 d experiment also become readily available, experiment need less than one week time.
To explore the low sensitivity to the samples
Large biological combination
~ 7.5 mg U - 13 c and 15 n mark Kif5b, 349 residual protein, and microtubules composite total sample size ~ 80 mg, by the United States, the state T.P ollenova professor.
Due to the sensitivity enhancement, more challenging samples (more complex or less markup) become the focus of researchers.
We record the 3 d NCACX and NCOCX experiment, the samples for a contains about 350 residues of unmarked marker protein and protein complexes (about 9% total quantity of isotope labeled substance).
The experiment lasted for about 5 and 6 days respectively, proved that the probe on the rf channel all at the same time illuminate accumulation under the multiple steps of the stability of a few days.
Biological samples in its native environment
Branching coli into enough cells coated
~ 40 mg of 13 c and 15 n labeled cell wall, 50 mm HEPES pH 7.0, by the French U.G renoble j. p. simorre professor
Because of the increase in the sensitivity of the researchers can directly by solid state nuclear magnetic resonance (NMR) research of the cell.
Unstable samples tends to rapid degradation over time, the probe for the sample of the unstable is a game changer, the key is to soon after samples generated collecting all the data.
Natural abundance of natural products
Wood and fiber
Wood from bordeaux, provided by the French bordeaux CNRS professor.
Timber and other samples that are rich in cellulose usually presents a mixture of amorphous and crystalline materials, so there will be a mixture of a large number of signals and narrow.In experiment 1 d 13 c to distinguish different overlapping spectral component is often not easy.Can improve resolution by 2 d CC related experiment is sometimes belonging spectra signal is the only feasible way.With the improvement of biological solid CryoProbe sensitivity, INADEQUATE reunion a conventional tool.
Natural abundance of natural products
Native collagen in the bone matrix
Goats femoral cortical bone (Capra hircus, 2-3 years old).Biomedical research center in India N.S inha.
To understand the structure of collagen in health and disease state and functional behavior, for all kinds of tissue engineering bone degenerative disease, and is a milestone in the development of bone implant therapy.Collagen usually have the natural abundance of spectrum sensitivity and limited isotope concentration.
Enhanced due to the sensitivity of the probe, can now be recorded in the natural isotopic abundance of collagen high resolution 2 d 1 h - 13 c HETCOR experiment.In a short time and long time under the contact time record of the spectrum, illustrates the natural environment in the real collagen short-range and long-range interaction in the bone matrix.Through the probe, the researchers learn more about the structural stability of collagen in bone matrix and function mechanism.
In situ characteristics of active pharmaceutical ingredients
Metal organic framework based on cyclodextrins (CD - MOFs)
CDMOF particles loaded with about 20% of Lansoprazole, by c. Martinau - professor Corcos, CEMHTI UPR CNRS 3079, ILV UMR CNRS IUF provide 8180 and France.
Dosing matrix are usually similar Yu Haimian porous materials.Metal organic framework (CD - MOF) is a very good example, because they are a huge gap of the material.Join the MOFs drug represents a dilution of the spin system, in this case, the sensitivity of the lack of in situ characterization of the active ingredient is a big problem.
It is worth noting that the low temperature sensor technology is so far the only allow the detection of such low content of API sample status tool.Other methods, such as rapid MAS 1 h NMR or DNP has proven unsuitable or use limited, because the solvent used for DNP sample preparation in the CD - MOF resolution is low and unstable.
Advanced characterization of API
Because the probe has the remarkable sensitivity, can in the case of without using isotope labeling for advanced characterization of API.It can be used under the natural abundance of vitamin B12 CC double quantum related to illustrate.Reunion INADEQUATE known as low sensitivity, need more than a month in RT probe acquisition time.
Based on the CP and double CP experiment
CPMAS CryoProbe is the standard in structural biology and advanced development of CP experiment.
The high sensitivity combined with NUS
New probe of high sensitivity combined with non-uniform sampling technology, can significantly shorten the time.CPMAS CryoProbe is limited sensitivity of sample data acquisition speed to speed up 10 times.
1.NPM1exhibitsstructuralThe andThe dynamicheterogeneityuponphaseSeparation.withthep14ARFtumorsuppressor
Eric Gibbs, Barbara Perrone, Alia Hassan, Rainer Kummerle, Richard Kriwacki.
Journal of Magnetic Resonance, 2020, 310, 10646
2.Sensitivity Boosts by the CPMASCryoProbeFor Challenging in Assemblies
Alia Hassan, Caitlin M.Q uinn, Jochem Struppe, Ivan v. ergeyev, Chunting Zhang, Changmiao Guo, Brent Runge, Theint Theint, Hanh H.D ao, Christopher p. Jaroniec, Melanie Berbon and Alons Lends, Birgit Habenstein, Antoine Loquet, Rainer Kuemmerle, Barbara Perrone, Angela Gronenborn, Tatyana Polenova.
Journal of Magnetic Resonance, 2020, 311, 106680
3.Efficient incorporation and the protection of lansoprazole in cyclodextrin metal - organic frameworks
Xue Li, Marianna Porcino, Charlotte Martineau Corcos, Tao Guo, Ting Xiong, Weifen Zhu, Gilles Patriarch, Christine Pechoux, Barbara Perrone, Alia Hassan, Rainer Kummerle, Alexandre Michelet, Anne Zehnacker - Rentien Jiwen Zhang Ruxandra Gref.
International Journal of Pharmaceutics, 2020, 585, 119442
4. Probing short and long - range interactions in native collagen inside the ipads matrix by BioSolids CryoProbe
Expand Tiwari, Sebastian Wegner, Alia Hassan, Navneet Dwivedi, RamaNand Rai, and Neeraj Sinha.
Accepted in Magnetic Resonance in Chemistry
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