Process for producing a complex of a lanthanide with a macrocyclic ligand
A technology of macrocyclic ligands and lanthanides, which can be used in pharmaceutical formulations, drug delivery, preparations for in vivo tests, etc.
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[0073] Measurement
[0074] Moisture content in DOTA
[0075] The measurement of the moisture content in DOTA was performed as described in Karl Fischer's semi-micro method (Fischer, Karl - Pharm. Eur. Section 2.5.12).
[0076] Analysis of free form of DOTA in solution (free DOTA)
[0077] Solution A: Dissolve 50 g of sodium acetate in 10 ml of glacial acetic acid and adjust the volume to 1000.0 ml with carbon dioxide-free water. The obtained solution was adjusted to pH (5±0.05) with 0.1 M sodium hydroxide solution or glacial acetic acid.
[0078] Solution B: Dissolve 50.8 mg of xylenol orange in carbon dioxide-free water and adjust the volume to 100.0 ml with the same solvent. Use freshly prepared solutions.
[0079] Solution C: 3 mL of Solution B was added to 30 mL of Solution A, and the volume of this solution was increased to 200.0 mL with carbon dioxide-free water.
[0080] A 0.005M solution of gadolinium sulfate was prepared as follows: 3.735 grams of gadolinium sul...
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