Journal
JOURNAL OF MAGNETIC RESONANCE
Volume 284, Issue -, Pages 115-124Publisher
ACADEMIC PRESS INC ELSEVIER SCIENCE
DOI: 10.1016/j.jmr.2017.09.013
Keywords
NMR; Hyperpolarization; Parahydrogen; C-13; Spectroscopy; Low field; Instrumentation
Funding
- NIH ICMIC [5P50 CA128323-03, 5R00 CA134749-03, 3R00CA134749-02S1]
- DoD (CDMRP Breast Cancer Program Era of Hope Award) [W81XWH-12-1-0159/BC112431]
- [1R21GM107947]
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Applications of parahydrogen induced polarization (PHIP) often warrant conversion of the chemically synthesized singlet-state spin order into net heteronuclear magnetization. In order to obtain optimal yields from the overall hyperpolarization process, catalytic hydrogenation must be tightly synchronized to subsequent radiofrequency (RF) transformations of spin order. Commercial NMR consoles are designed to synchronize applied waves on multiple channels and consequently are well-suited as controllers for these types of hyperpolarization experiments that require tight coordination of RF and non-RF events. Described here is a PHIP instrument interfaced to a portable NMR console operating with a static field electromagnet in the milliTesla regime. In addition to providing comprehensive control over chemistry and RF events, this setup condenses the PHIP protocol into a pulse-program that in turn can be readily shared in the manner of traditional pulse sequences. In this device, a TTL multiplexer was constructed to convert spectrometer TTL outputs into 24 VDC signals. These signals then activated solenoid valves to control chemical shuttling and reactivity in PHIP experiments. Consolidating these steps in a pulse programming environment speeded calibration and improved quality assurance by enabling. the B-0/B-1, fields to be tuned based on the direct acquisition of thermally polarized and hyperpolarized NMR signals. Performance was tested on the parahydrogen addition product of 2-hydroxyethyl propionate-1-C-13-d(3), where the C-13 polarization was estimated to be P-13c = 20 +/- 2.5% corresponding to C-13 signal enhancement approximately 25 million-fold at 9.1 mT or approximately 77,000-fold C-13 enhancement at 3 T with respect to thermally induced polarization at room temperature. (c) 2017 Elsevier Inc. All rights reserved.
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