4488
M. D. Moran et al. / Bioorg. Med. Chem. 20 (2012) 4482–4488
6. Katsifis, A.; Kassiou, M. Mini-Rev Med Chem 2004, 4, 909.
4.5. Ex vivo biodistribution
7. Sieghart, W. J. Psychiatr. Neurosci. 1994, 19, 24.
8. Sieghart, W. Pharmacol. Rev. 1995, 47, 181.
Preliminary ex vivo biodistribution studies of [11C]4, [11C]5, and
9. Korpi, E. R.; Matilla, M. J.; Wisden, W.; Luddens, H. Ann. Med. 1997, 29, 275.
10. Atack, J. R. Curr. Drug Targets CNS Neurol. Disord. 2003, 2, 213.
11. Maziere, M.; Hantraye, P.; Prenant, C. H.; Sastre, J.; Comar, D. Int. J. Appl. Radiat.
Isot. 1984, 35, 973.
12. Hammers, A. Neuroimag. Clin. N. Am. 2004, 14, 537.
13. Halldin, C.; Stone-Elander, S.; Thorell, J.-O.; Persson, A.; Sedvall, G. J. Radiat.
Appl. Instrum. Part A 1988, 39, 993.
14. Ryzhikov, N. N.; Seneca, N.; Krasikova, R. N.; Gomzina, N. A.; Shchukin, E.;
Fedorova, O. S.; Vassiliev, D.; Gulyás, B.; Hall, H.; Savic, I.; Halldin, C. Nucl. Med.
Biol. 2005, 32, 109.
15. Odano, I.; Halldin, C.; Karlsson, P.; Varrone, A.; Airaksinen, A. J.; Krasikova, R.
N.; Farde, L. NeuroImage 2009, 45, 891.
[
11C]6 in conscious male Sprague-Dawley rats were conducted
(n = 1 rat per time point) as previously described.40,48 For the full
biodistribution study, all rats received ca. 37 MBq (1 mCi) of
[
11C]5 in 0.3 mL of buffered saline (containing 10% ethanol) via
the tail vein and were sacrificed by decapitation at either 5, 15,
30 or 60 min after injection (n = 4 per time point). The brains were
removed, and regions of interest were excised, blotted, weighed
and then counted for radioactivity (Table 1).
16. Beer, H. F.; Blauenstein, P. A.; Hasler, P. H.; Delaloye, B.; Ricabona, G.; Bangerl, I.;
Hunkeler, W.; Bonetti, E. P.; Piere, L.; Richards, J. G. J. Nucl. Med. 1990, 31, 1007.
17. Westera, G.; Buck, A.; Burger, C.; Leenders, K. L.; von Schulthess, G. K.;
Schubinger, A. P. Eur. J. Nucl. Med. 1996, 23, 5.
18. Halldin, C.; Farde, L.; Litton, J.-E.; Hall, H.; Sedvall, G. Psychopharmacology 1992,
108, 16.
19. Lingford-Hughes, A.; Hume, S. P.; Feeney, A.; Hirani, E.; Osman, S.;
Cunningham, V. J.; Pike, V. W.; Brooks, D. J.; Nutt, D. J. J. Cereb. Blood Flow
Metab. 2002, 22, 878.
20. Maeda, J.; Suhara, T.; Kawabe, K.; Okauchi, T.; Obayashi, S.; Hojo, J.; Suzuki, K.
Synapse 2003, 47, 200.
4.6. Blocking studies
Rats received intraperitoneal injections of a solution (0.4–
0.6 mL) of 5% DMSO/5% EtOH in saline (containing 5% Tween80
w/w; vehicle), 0.1 mg/kg of 5, 5 mg/kg of 5, or 10 mg/kg of flu-
mazenil at 30 min before administration of [11C]5. Using the proto-
col described above, rats were sacrificed and dissected at 15 min
post-injection of the radiotracer (Table 2).
21. Coenen, H. H.; Moerlein, S. M. J. Fluorine Chem. 1987, 36, 63.
22. Grunder, G.; Siessmeier, T.; Lange-Asschenfeldt, C.; Vernaleken, I.; Buchholz, G.
G.; Stoeter, P.; Drzezga, A.; Luddens, H.; Rösch, F.; Bartenstein, P. Eur. J. Nucl.
Med. 2001, 28, 1463.
4.7. Metabolism studies
Following tail-vein injection of [11C]5, as described above,
whole blood was collected at 5 and 15 min from the trunk in a hep-
arinized tube and centrifuged. The plasma was analyzed by radio-
HPLC using the method of Hilton and coworkers,49 with minor
modifications.50 Briefly, rat plasma from either time point was di-
rectly loaded onto a 5 mL HPLC injector loop and injected onto a
capture column (4.6 mm  20 m) that was packed in-house with
23. Todde, S.; Moresco, R. M.; Fröstl, W.; Stampf, P.; Matarrese, M.; Carpinelli, A.;
Magni, F.; Kienle, M. G.; Fazio, F. Nucl. Med. Biol. 2000, 27, 565.
24. Prenant, C.; Crouzel, C.; Valois, J. M.; Robertson, D. W.; Comar, D. Appl. Radiat.
Isot. Int. J. Radiat. Appl. Instrum. Part A 1992, 43, 946–948.
25. Maziere, M.; Godot, J.-M.; Berger, G.; Prenant, C. H.; Comar, D. J. Radioanal.
Chem. 1980, 56, 229.
26. Ishiwata, K.; Yanai, K.; Ido, T.; Miura-Kanno, Y.; Kawashima, K. J. Radiat. Appl.
Instrum. Part B 1988, 15, 365.
27. Johnströma, P.; Stone-Elander, S.; Buelfer, T. J. Labelled Compd. Radiopharm.
1994, 34, 147.
28. Alhambra, C.; Becker, C.; Blake, T.; Chang, A.; Damewood, J. R. J.; Daniels, T.;
Dembofsky, B. T.; Gurley, D. A.; Hall, J. E.; Herzog, K. J.; Horchler, C. L.;
Ohnmacht, C. J.; Schmiesing, R. J.; Dudley, A.; Ribadeneira, M. D.;
Knappenberger, K. S.; Maciag, C.; Stein, M. M.; Chopra, M.; Liu, X. F.;
Christian, E. P.; Arriza, J. L.; Chapdelaine, M. J. Bioorg. Med. Chem. 2011, 19,
2927.
OASIS HLB 30 lm (Waters, NJ). The capture column was eluted
with 1% aqueous CH3CN (2 mL/min) for approximately 3 min and
À
then back-flushed with 50:50 CH3CN/H2O + 0.1 N NH4+HCO2 (pH
4); 2.0 mL/min onto
a
Phenomenex Luna C18 Column
(250 Â 4.6 mm, 10
l
). The column effluents from both columns
29. Chang, H.-F.; Chapdelaine, M. J.; Dembofsky, B. T.; Herzog, K. J.; Horchler, C.;
Schmiesing, R. J. 2008. WO Patent 2008/155572 A2.
were monitored through a flow detector (Bioscan Flow-Count)
operated in coincidence mode. Whole brain from a control rat
30. Orrù, A.; Lai, P.; Lobina, C.; Maccioni, P.; Piras, P.; Scanu, L.; Froestl, W.; Gessa,
G. L.; Carai, M. A. M.; Colombo, G. Eur. J. Pharmacol. 2005, 525, 105.
31. Liang, J.-H.; Chen, F.; Krstew, E.; Cowen, M. S.; Carroll, F. Y.; Crawford, D.; Beart,
P. M.; Lawrence, A. J. Neuropharmacology 2006, 50, 632.
32. Slattery, D. A.; Markou, A.; Froest, W.; Cryan, J. F. Neuropsychopharmacology
2005, 30, 2065.
33. Tsai, M.-L.; Shen, B.; Leung, L. S. Epilepsy Res. 2008, 79, 187.
34. Kato, K.; Zhang, M.-R.; Suzuki, K. Bioorg. Med. Chem. Lett. 2009, 19, 6222.
35. Kerr, D. I. B.; Ong, J.; Perkins, M. V.; Prager, R. H.; Puspawati, N. M. Aust. J. Chem.
2006, 59, 445.
was removed and treated with ca. 1.3 MBq (37 l
Ci) of [11C]5, and
the whole brain was removed from rats sacrificed at 5 or 15 min
post-injection. Brains were individually homogenized with ice-
cold 80:20 CH3CN/H2O + 0.01 N HCl and centrifuged as previously
described by our laboratory,50 prior to radio-HPLC analysis of the
supernatant using the aforementioned method.
Acknowledgements
36. Hopkins, G. C.; Jonak, J. P.; Minnemeyer, H. J.; Tieckelmann, H. J. Org. Chem.
1967, 32, 4040.
37. Singh, B. K.; Cavalluzzo, C.; Maeyer, M. D.; Debyser, Z.; Parmar, V. S.; Eycken, E.
V. D. Synthesis 2009, 8, 2725.
38. Wilson, A. A.; Garcia, A.; Jin, L.; Houle, S. Nucl. Med. Biol. 2000, 27, 529.
39. Wilson, A. A.; Garcia, A.; Houle, S.; Vasdev, N. J. Labelled Compd. Radiopharm.
2009, 52, 490.
40. Vasdev, N.; Natesan, S.; Galineau, L.; Garcia, A.; Stableford, W. T.; McCormick,
P.; Seeman, P.; Houle, S.; Wilson, A. A. Synapse 2006, 60, 314.
41. Wong, D. F.; Pomper, M. G. Mol. Imag. Biol. 2003, 5, 350.
42. Waterhouse, R. N. Mol. Imaging Biol. 2003, 5, 376.
43. Wilson, A. A.; Jin, L.; Garcia, A.; DaSilva, J. N.; Houle, S. Appl. Radiat. Isot. 2001,
54, 203.
The authors thank Armando Garcia, Winston Stableford and
Min Wong for assistance with the radiochemisty, and Justin Hicks
for assistance with the logD7.4 determinations. CAMH is gratefully
acknowledged for support in the form of a post-doctoral fellowship
(M.D.M.).
Supplementary data
44. Pirker, S.; Schwarzer, C.; Wieselthaler, A.; Sieghart, W.; Sperk, G. Neuroscience
2000, 101, 815.
45. Pike, V. W. Trends Pharmacol. Sci. 2009, 30, 431.
Supplementary data associated with this article can be found, in
46. Crouzel, C.; Långström, B.; Pike, V. W.; Coenen, H. H. Appl. Radiat. Isot. Int. J.
Radiat. Appl. Instrum. Part A 1987, 38, 601.
47. van Oosten, E. M.; Wilson, A. A.; Stephenson, K. A.; Mamo, D. C.; Pollock, B. G.;
Mulsant, B. H.; Yudin, A. K.; Houle, S.; Vasdev, N. Appl. Radiat. Isot. 2009, 67,
611.
48. Wilson, A. A.; DaSilva, J. N.; Houle, S. Nucl. Med. Biol. 1996, 23, 141.
49. Hilton, J.; Yokoi, F.; Dannals, R. F.; Ravert, H. T.; Szabo, Z.; Wong, D. F. Nucl. Med.
Biol. 2000, 27, 627.
50. Wilson, A. A.; Garcia, A.; Parkes, J.; McCormick, P.; Stephenson, K. A.; Houle, S.;
Vasdev, N. Nucl. Med. Biol. 2008, 35, 305.
References and notes
1. Nutt, D. J.; Malizia, A. L. Br. J. Psychiatry 2001, 179, 390.
2. Mehta, A. K.; Ticku, M. K. Brain Res. Rev. 1999, 29, 196.
3. Jakobsen, S.; Kodahl, G. M.; Olsen, A. K.; Cumming, P. Nucl. Med. Biol. 2006, 33,
593.
4. Rudolph, U.; Möhler, H. Annu. Rev. Pharmacol. Toxicol. 2004, 44, 475.
5. Krystal, J. H.; Staley, J.; Mason, G.; Petrakis, I. L.; Kaufman, J.; Harris, R. A.;
Gelernter, J.; Lappalainen, J. Arch. Gen. Psychiatry 2006, 63, 957.