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Refining method of crude tacrolimus

A technique for the purification of tacrolimus, which is applied in the field of purification of tacrolimus by reversed-phase high-performance liquid phase preparative chromatography, and the field of purification of tacrolimus, a potent immunosuppressant of macrolides, can solve the problem of purification and collection. Low rate, patient burden, high cost and other problems, to achieve the effect of high purity

Active Publication Date: 2010-05-26
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These patents reported the use of adsorption resin or modified silica gel to purify tacrolimus, the purification yield is low, resulting in high cost of products after industrial production, causing heavy burden to patients

Method used

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Examples

Experimental program
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Effect test

example 1

[0033] Weigh 10 g of crude tacrolimus, dissolve it in 50 mL of acetonitrile-water (60:40), and filter it with a 0.45 μm filter membrane. The mobile phase is acetonitrile-water, the flow rate is 20mL / min, and the column temperature is 25°C. After the chromatograph equilibrates the baseline with acetonitrile-water (75:25), inject 1mL of the sample and wash it with acetonitrile-water (75:25) first. Remove 2-3 column volumes, then use acetonitrile-water (60:40) to elute 2-3 column volumes, then use acetonitrile-water (55:45) to elute 3-5 column volumes, and finally use Acetonitrile-water (45:55) was eluted for 5-6 column volumes, and the eluate containing high-purity tacrolimus was collected according to the peak conditions.

[0034] The collected liquids were combined and concentrated under reduced pressure until there was no acetonitrile, and the concentrated liquid was extracted twice with ethyl acetate, and the extracted ethyl acetate layer was concentrated under reduced press...

example 2

[0036] Weigh 10 g of crude tacrolimus, dissolve it in 50 mL of acetonitrile-tetrahydrofuran-water (40:40:20), and then filter through a 0.45 μm filter membrane. The mobile phase was acetonitrile-tetrahydrofuran-water, the flow rate was 15 mL / min, the column temperature was 25° C., and the detection wavelength was 230 nm. After equilibrating the baseline of the chromatograph with acetonitrile-tetrahydrofuran-water (40:40:20), inject 1 mL, first elute with acetonitrile-tetrahydrofuran-water (40:40:20) for 2-3 column volumes, and then use acetonitrile-tetrahydrofuran-water (40:40:20) to elute Tetrahydrofuran-water (30:35:35) was eluted for 2-3 column volumes, followed by acetonitrile-tetrahydrofuran-water (25:30:45) for 2-3 column volumes, and finally acetonitrile-tetrahydrofuran-water ( 25:25:50) to elute 5-6 column volumes, collect and combine the eluate containing high-purity tacrolimus according to the peak conditions.

[0037] Combine the collected solution and concentrate ...

example 3

[0039]Weigh 10 g of crude tacrolimus, dissolve it in 50 mL of methanol-acetonitrile-water (40:45:15), and filter it through a 0.45 μm filter membrane. The mobile phase of the chromatograph is methanol-acetonitrile-water, the flow rate is 15mL / min, the column temperature is 25°C, and the detection wavelength is 230nm. After equilibrating the baseline of the chromatograph with methanol-acetonitrile-water (40:45:15), inject 1 mL of the sample, first elute with methanol-acetonitrile-water (40:45:15) for 2-3 column volumes, and then use methanol- Acetonitrile-water (35:40:25) was eluted for 2-3 column volumes, followed by methanol-acetonitrile-water (30:40:30) for 2-3 column volumes, and finally methanol-acetonitrile-water ( 30:30:40) to elute for 6-8 column volumes, collect and combine the eluate containing high-purity tacrolimus according to the peak conditions.

[0040] Combine the collected solution and concentrate under reduced pressure until there is no acetonitrile and meth...

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Abstract

The invention belongs to the technical field of medicinal biotechnology field, specifically relates to a refining method of macrolide powerful immunosuppressant tacrolimus and in particular to a method for refining tacrolimus through reversed-phase high performance liquid preparative chromatography. The method uses crude tacrolimus as raw material to dissolve in organic solvent and adopts C18 reversed-phase preparative liquid chromatography to realize the separation and purification of tacrolimus, ascomycin and dihydro-tacrolimus. The refining method of the invention adopts the proper elution system and has good stability, the impurities can be completely separated under the condition of preparative chromatography, the primary loading quantity can be 200mg, the purity of the obtained tacrolimus can be over 98.5% through HPLC detection; and the whole refining process has simple operation and good universality, is easy to popularize and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of medicine and biology, and in particular relates to a method for refining tacrolimus, a potent immunosuppressant of macrolides, in particular to a method for refining tacrolimus by reverse-phase high-performance liquid phase preparation chromatography. Background technique [0002] Over the past ten years, organ transplantation in my country has developed rapidly, ranking first in Asia and second in the world. Immunosuppressant drugs used to reduce rejection after organ transplantation are also showing a rapid growth trend. The immunosuppressant commonly used to prevent and suppress rejection is cyclosporine, but its side effects are large, which has brought great harm to the majority of patients. A certain pain. [0003] Tacrolimus, also known as FK-506, is a macrolide antibiotic extracted from soil actinomycetes by Fujisawa Pharmaceutical Company of Japan in 1984. It has strong immunosuppressive propert...

Claims

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Application Information

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IPC IPC(8): C07D498/18B01D15/08
Inventor 刘忠
Owner LUNAN PHARMA GROUP CORPORATION
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