反应详情

温度

95 °C

Radiolabeling was performed following a literature procedure (Wang et al., Nature Protocols, vol. 1, pp. 1477-1480, 2006). Briefly, 1 mg (75.3 mmol) of compound SRVI34 was dissolved in 1 ml of 0.5 M ammonium acetate buffer at pH 8. Disodium tartarate dihydrate was dissolved in the labelling buffer of 0.5 M ammonium acetate (pH 8) to a concentration of 50 mg/ml. Ascorbic acid-HCl solution was prepared by dissolving ascorbic acid in 10 mM HCl to a concentration of 1.0 mg/ml. A solution of SRVI34 (80 μl) was combined to a solution of 45 μl 0.25 M ammonium acetate, 15 μl tartarate buffer, followed by 5 μl of the freshly prepared 4 mg/ml SnCl2. 2H2O solution in the ascorbate-HCl solution. The final pH will be about 8-8.5. After vortexing, was added 20 mCi of 99mTc-pertechnetate in 200 μl saline and was heated the solution at 90-100° C. for 20 min. Reaction mixture was cooled, diluted 850 μl of water and purified by HPLC using a Phenomenex C18 Luna 10×250 mm2 column on a Waters 600E Delta LC system with a Waters 486 tunable absorbance UV/Vis detector, both controlled by Empower software. HPLC solvent system, flow rate=4 ml/min, a gradient, 0-5 min, 80/20 water/acetonitrile (0.1% TFA in each solvent), 5-25 min 40/60 water/acetonitrile (0.1% TFA in each solvent) and 25-35 min 80/20 (0.1% TFA in each solvent) was used. Two radiolabeled products were found, called as [99mTc]SRVI34A (5.52 mCi) (retention time 17.5 min) and [99mTc]SRVI34B (6 mCi) (retention time 18.9 min) SRVI34A and SRVI32B are diastereomers, syn and anti-isomers with respect to the Tc═O group. Each product was neutralized with 50 μl of 1 M sodium bicarbonate and evaporated to dryness under vacuum. The obtained solid residues was dissolved in 200 μl saline and used for imaging and biodistribution studies.

1. customReaction mixture
2. temperaturewas cooled
3. custompurified by HPLC
4. customa gradient, 0-5 min, 80/20 water/acetonitrile
5. custom5-25 min 40/60 water/acetonitrile
6. custom25-35 min 80/20
7. customevaporated to dryness under vacuum
8. dissolutionThe obtained solid residues was dissolved in 200 μl saline