We
present on the utility of in situ nuclear magnetic resonance
(NMR) and near-infrared (NIR) spectroscopic techniques for automated
advanced analysis of the 129Xe hyperpolarization process
during spin-exchange optical pumping (SEOP). The developed software
protocol, written in the MATLAB programming language, facilitates
detailed characterization of hyperpolarized contrast agent production
efficiency based on determination of key performance indicators, including
the maximum achievable 129Xe polarization, steady-state
Rb–129Xe spin-exchange and 129Xe polarization
build-up rates, 129Xe spin-relaxation rates, and estimates
of steady-state Rb electron polarization. Mapping the dynamics of 129Xe polarization and relaxation as a function of SEOP temperature
enables systematic optimization of the batch-mode SEOP process. The
automated analysis of a typical experimental data set, encompassing
∼300 raw NMR and NIR spectra combined across six different
SEOP temperatures, can be performed in under 5 min on a laptop computer.
The protocol is designed to be robust in operation on any batch-mode
SEOP hyperpolarizer device. In particular, we demonstrate the implementation
of a combination of low-cost NIR and low-frequency NMR spectrometers
(∼$1,100 and ∼$300 respectively, ca. 2020) for use in
the described protocols. The demonstrated methodology will aid in
the characterization of NMR hyperpolarization hardware in the context
of SEOP and other hyperpolarization techniques for more robust and
less expensive clinical production of HP 129Xe and other
contrast agents.