Preparation method of pristinamycin IA mono-component
A ponamycin, single-component technology, applied in the preparation of pharmaceutical raw materials, the field of single-component preparation of ponamycin IA, can solve the problems of difficult industrialized production of products, high process costs, inability to overcome purification steps, and the like, To achieve the effect of easy operation, strong controllability and short process flow
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Embodiment 1
[0024] a. The crude product of prunamycin IA (see the attached figure 1 ) 5.0g, dissolved in 25mL of acetonitrile to obtain the sample solution.
[0025] b. The sample solution was injected into a chromatographic column equipped with C18 filler, and a binary liquid phase separation system was used to elute with 38% acetonitrile-acid water (0.4‰ acetic acid), and the eluate with an HPLC content greater than 98.5% was collected.
[0026] c. The eluate was concentrated under reduced pressure at 30° C., and the organic solvent was evaporated to obtain a prunamycin IA concentrate. The concentrated solution was filtered and washed with water to obtain prunamycin IA wet powder. Put the wet powder in an oven with a vacuum degree of ≥0.08Mpa at 40°C, and dry it in vacuum for 5 hours to obtain the refined product of prunamycin IA (see the attached figure 2 ) 2.6g, the purity is 98.6%, and the preparation yield is 76.4%.
Embodiment 2
[0028] a. 25g of prunamycin IA crude product was dissolved in 250mL of DMF to obtain the loading solution.
[0029] b. The sample solution was injected into a chromatographic column equipped with C18 filler, and a binary liquid phase separation system was used to elute with 40% acetonitrile-acidic water (0.5‰ acetic acid), and the eluate with an HPLC content greater than 98.5% was collected.
[0030] c. The eluate was concentrated under reduced pressure at 40°C, and the organic solvent was evaporated to obtain the prunamycin IA concentrate. The concentrated solution was filtered and washed with water to obtain prunamycin IA wet powder. The wet powder was placed in an oven at 45°C with a vacuum degree of ≥0.08Mpa, and vacuum-dried for 8 hours to obtain 12.8g of prunamycin IA refined product with a purity of 99.1% and a preparation yield of 75.6%.
Embodiment 3
[0032] a. 100 g of prunamycin IA crude product was dissolved in 300 mL of DMF to obtain the loading solution.
[0033] b. The sample solution was injected into a chromatographic column equipped with C18 filler, and a binary liquid phase separation system was used to elute with 42% acetonitrile-acidic water (0.6‰ formic acid), and the eluate with an HPLC content greater than 98.5% was collected.
[0034] c. The eluate was concentrated under reduced pressure at 50° C., and the organic solvent was evaporated to obtain a prunamycin IA concentrate. The concentrated solution was filtered and washed with water to obtain prunamycin IA wet powder. The wet powder was placed in an oven at 45°C with a vacuum degree of ≥0.08Mpa, and vacuum-dried for 12 hours to obtain 52g of refined prunamycin IA with a purity of 98.9% and a preparation yield of 76.6%.
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