Purification method of gadobutrol
A purification method, the technology of gadobutrol, applied in the field of medicine, can solve the problems of low degree of automation, cumbersome purification process, affecting production efficiency, etc., and achieve the effect of high degree of automation, less purification loss and prolonging the service life
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Embodiment 1
[0027] Step 1: Preparation of crude gadobutrol
[0028] 100kg of purified water was pumped into the 200L reactor, 9.4kg of concentrated hydrochloric acid was added to stir, 17kg of gadolinium oxide was added to stir, then 50kg of butanol ligand was added, and the reaction solution was heated to 90°C under stirring. 25°C, filter under pressure, and wash with appropriate amount of water. The filtrate containing the product gadobutrol is demineralized by nanofiltration until the conductivity of the solution at the outlet of the waste liquid drops to 100-200 μs / cm. At this time, the conductivity of the feed liquid after nanofiltration is 1300 μs / cm, and the nanofiltration result is transferred to 500L reaction kettle, concentrated under reduced pressure to an internal weight of about 125kg. Yield 90.4%
[0029] Step 2: Preparation of Gadobutrol Finished Products
[0030] Packing, two FPA53 type anion exchange resin columns, one IR-120H type cation exchange resin column: diamete...
Embodiment 2
[0035] Gadobutrol Finished Product Preparation and Resin Bed Reuse:
[0036] The resin column used in Example 1 is activated by acid and alkali again after purifying gadobutrol (FPA53 type anion exchange resin: pure water rinses the resin column, 21 kg of 10% NaOH aqueous solution is slowly rinsed, pure water rinses the resin column until the conductivity of the clean water flowing out of the resin. Less than 40μS / cm.IR-120H type cation exchange resin: pure water rinses the resin column, 21kg of 5% HCl aqueous solution slowly rinses, pure water rinses the resin column until the conductivity of the clean water flowing out of the resin is less than 10μS / cm).
[0037] Another batch of 33kg gadobutrol crude concentrate prepared according to the method of Example 1 was eluted using the anion-yang-anion three resin columns that were repeatedly activated, and then 33kg purified water was used to rinse the resin bed to collect the final eluent , the water washing solution was concentr...
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