A highly versatile automatized setup for quantitative measurements of PHIP enhancements

Kiryutin, Alexey S.; Sauer, Grit; Hadjiali, Sara; Yurkovskaya, Alexandra V.; Breitzke, Hergen; Buntkowsky, Gerd

doi:10.1016/j.jmr.2017.10.007

Cited by 47 publications

(45 citation statements)

References 54 publications

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“…NMR System and Experimental Setup : Experiments were performed on an NMR spectrometer (Avance III HD 300 MHz, Bruker, Germany) using a dual‐channel 1 H/broad band probe head (5 mm PA BBO 300S1 BBF‐H‐D‐05‐Z) at a magnetic field of 7 T. The setup follows an idea similar to a setup described before (denoted by setup 3 ).…”

Section: Methodsmentioning

confidence: 99%

SAMBADENA Hyperpolarization of ¹³C‐Succinate in an MRI: Singlet‐Triplet Mixing Causes Polarization Loss

Berner

Schmidt²,

Zimmermann

et al. 2019

ChemistryOpen

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The signal enhancement provided by the hyperpolarization of nuclear spins of biological molecules is a highly promising technique for diagnostic imaging. To date, most 13C‐contrast agents had to be polarized in an extra, complex or cost intensive polarizer. Recently, the in situ hyperpolarization of a 13C contrast agent to >20 % was demonstrated without a polarizer but within the bore of an MRI system. This approach addresses some of the challenges of MRI with hyperpolarized tracers, i. e. elevated cost, long production times, and loss of polarization during transfer to the detection site. Here, we demonstrate the first hyperpolarization of a biomolecule in aqueous solution in the bore of an MRI at field strength of 7 T within seconds. The 13C nucleus of 1‐13C, 2,3‐2H2‐succinate was polarized to 11 % corresponding to a signal enhancement of approximately 18.000. Interesting effects during the process of the hydrogenation reaction which lead to a significant loss of polarization have been observed.

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Section: Methodsmentioning

confidence: 99%

SAMBADENA Hyperpolarization of ¹³C‐Succinate in an MRI: Singlet‐Triplet Mixing Causes Polarization Loss

Berner

Schmidt²,

Zimmermann

et al. 2019

ChemistryOpen

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“…As as tartingp oint, we optimized the experimental conditions for the hyperpolarization of the alkyne-bearing peptide sample. In particular,w ee mployed 90 %p ara-H 2 enriched hydrogen at ap ressure of 3bar,w ith at ailoredd issolution time of 10 s. [12] Hydrogenation took place inside the magnet under PASADENA [4b] conditions resulting in af ast PHIP pre-hyperpolarization. Figure 1c ompares the thermal 1 HNMR spectrum before and after hydrogenation with the respective PHIP one.…”

mentioning

confidence: 99%

Ultrafast Single‐Scan 2D NMR Spectroscopic Detection of a PHIP‐Hyperpolarized Protease Inhibitor

Kiryutin

Sauer

Tietze

et al. 2019

Chemistry A European J

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Two‐dimensional NMR spectroscopy is one of the most important spectroscopic tools for the investigation of biological macromolecules. However, due to the low sensitivity of NMR spectroscopy, it takes usually from several minutes to many hours to record such spectra. Here, the possibility of detecting a bioactive derivative of the sunflower trypsin inhibitor‐1 (SFTI‐1), a tetradecapeptide, by combining parahydrogen‐induced polarization (PHIP) and ultrafast 2D NMR spectroscopy is shown. The PHIP activity of the inhibitor was achieved by labeling with O‐propargyl‐l‐tyrosine. In 1D PHIP experiments a signal enhancement of a factor of approximately 1200 compared to standard NMR was found. This enhancement permits measurement of 2D NMR correlation spectra of low‐concentrated SFTI‐1 in less than 10 seconds, employing ultrafast single‐scan 2D NMR detection. As experimental examples PHIP‐assisted ultrafast single‐scan TOCSY spectra of SFTI‐1 are shown.

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“…Here we run experiments both at the high magnetic field of an NMR spectrometer, as well as at variable fields by using a fieldcycling NMR device described earlier. [10] Our experiments clearly demonstrate that the two protons of the thiophene derivative under study have a long-lived state with a lifetime of approximately 120 s in D 2 O, increasing to 240 s in deuterated methanol. Furthermore, in Cl-TC one can excite an LLC with an astonishingly long decoherence time of about 30 s. Very similar results were obtained also for bromothiophene carboxylate (Br-TC, not shown here).…”

Section: Introductionmentioning

confidence: 56%

Proton Relaxometry of Long‐Lived Spin Order

et al. 2019

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A study of long‐lived spin order in chlorothiophene carboxylates at both high and low magnetic fields is presented. Careful sample preparation (removal of dissolved oxygen in solution, chelating of paramagnetic impurities, reduction of convection) allows one to obtain very long‐lived singlet order of the two coupled protons in chlorothiophene derivatives, having lifetimes of about 130 s in D2O and 240 s in deuterated methanol, which are much longer than the T1‐relaxation times (18 and 30 s, respectively, at a field B0 =9.4 T). In protonated solvents the relaxation times become shorter, but the lifetime is still substantially longer than T1 . In addition, long‐lived coherences are shown to have lifetimes as long as 30 s. Thiophene derivatives can be used as molecular tags to study slow transport, slow dynamics and slow chemical processes, as has been shown in recent years.

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A highly versatile automatized setup for quantitative measurements of PHIP enhancements

Cited by 47 publications

References 54 publications

SAMBADENA Hyperpolarization of ¹³C‐Succinate in an MRI: Singlet‐Triplet Mixing Causes Polarization Loss

SAMBADENA Hyperpolarization of ¹³C‐Succinate in an MRI: Singlet‐Triplet Mixing Causes Polarization Loss

Ultrafast Single‐Scan 2D NMR Spectroscopic Detection of a PHIP‐Hyperpolarized Protease Inhibitor

Proton Relaxometry of Long‐Lived Spin Order

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A highly versatile automatized setup for quantitative measurements of PHIP enhancements

Cited by 47 publications

References 54 publications

SAMBADENA Hyperpolarization of 13C‐Succinate in an MRI: Singlet‐Triplet Mixing Causes Polarization Loss

SAMBADENA Hyperpolarization of 13C‐Succinate in an MRI: Singlet‐Triplet Mixing Causes Polarization Loss

Ultrafast Single‐Scan 2D NMR Spectroscopic Detection of a PHIP‐Hyperpolarized Protease Inhibitor

Proton Relaxometry of Long‐Lived Spin Order

Contact Info

Product

Resources

About

SAMBADENA Hyperpolarization of ¹³C‐Succinate in an MRI: Singlet‐Triplet Mixing Causes Polarization Loss

SAMBADENA Hyperpolarization of ¹³C‐Succinate in an MRI: Singlet‐Triplet Mixing Causes Polarization Loss