study were obtained from Sigma Aldrich (St. Louis, MO) or Fisher Scientific
(Pittsburgh, PA). Buffers used for radiolabeling were prepared in
chelexed Milli-Q water which was filtered through a 0.22 μm
nylon filter. A Varian Mercury-300 spectrometer or a VARIAN UNITY
Inova 400 spectrometer was utilized to record 1H (300 MHz)
NMR spectra. A VARIAN VXR 500 with a UNITY INOVA Console spectrometer
was used to record 13C (126 MHz) NMR spectra. Chemical
shifts are reported in parts per million and referenced to residual
solvent resonance peaks. Radio-TLC detection was accomplished using
a Bioscan 200 imaging scanner (Bioscan, Inc., Washington, DC). Radioactive
samples were counted on a Beckman Gamma 8000 counter containing a
NaI crystal (Beckman Instruments, Inc., Irvine, CA). A two-solvent
reversed-phase HPLC system was used to evaluate the radiolabeling
efficiency with water [0.05% trifluoroacetic acid (TFA)] and acetonitrile
(0.05% TFA). HPLC used a Kinetex (Phenomenex) C-18 column (5 μm,
4.6 × 150 mm I.D.). The HPLC instrument was composed of UV absorbance
detectors set at 220 and 280 nm, a NaI radiotracer detector, and a
photodiode array detector. A gradient elution with acetonitrile (0.1%
TFA) 0–100% buffer mobile phase over the course of 13 min and
a 1 mL/min flow rate was developed for radiochemical purity profiling.