Introduction of the purification process of rapamycin Rapamycin-RAPA

The molecular formula of rapamycin is C51H79NO13, the molecular weight is 914.172 g/mol, it is a white solid crystal, the melting point is 183-185 ° C, lipophilic, dissolved in organic solvents such as methanol , ethanol , acetone , chloroform, etc., very slightly soluble in water, almost Do not dissolve in ether. From the current animal experiment and clinical application, rapamycin is a new type of immunosuppressive agent with good curative effect, low toxicity and no nephrotoxicity.

There are large and small impurities in the crude product, and it is known that the after-hybrid is still an isomer, which is difficult to remove, and the total purity is 76.9%.

After the preliminary treatment of the crude product, the medium pressure preparation is carried out to obtain a preparation map:

The preparation is a double-pump medium-pressure system, which is characterized in that it can maintain the A and B flow ratios at the moment when the peak is eluted (the black line after 100 minutes in the figure is the peak). When, keep this degree, separate the front and back)

The highest absorption peak in the spectrum was collected step by step, and the purity was determined by analytical methods:

It was found that there was a sample with a purity of 97.2% in the collected liquid, which played a good role in removing impurities for the next step of refining.

Summary: The crude isomer impurities are large, which affects the delicate process in the later stage. Purification by one-step medium pressure can reduce the proportion of isomers. For the analysis of crude and prepared samples, it can be seen that the content of isomers is from 9.63% to 2.7%, and the purity of samples is improved from 76.9%. To 97.2%, to achieve the purpose of the experiment.