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Purifying and refining method of carbetocin

A carbetocin, purification and refining technology, applied in the field of drug purification and refining, can solve the problems of high single impurity content and low purification purity

Pending Publication Date: 2021-08-27
CISEN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Therefore, the technical problem to be solved in the present invention is to overcome the defects of low purification purity and high single impurity content of carbetocin in the prior art, thereby providing a kind of purification and refining method of carbetocin, through specific solvent High-purity carbetocin was obtained by beating, reverse-phase preparation, high-performance liquid chromatography, and two purification preparations.

Method used

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  • Purifying and refining method of carbetocin
  • Purifying and refining method of carbetocin
  • Purifying and refining method of carbetocin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Weigh 10.0g of crude carbetocin, add it to 50ml of methyl tert-butyl ether, beat at room temperature for 2 hours, use a sand core funnel to filter, and dry the filter cake at 20-30°C for 2 hours to obtain carbetocin. Crude oxytocin I.

[0042] (2) Add the above-mentioned carbetocin crude product I to 50ml of 95% ethanol, beat at room temperature for 2 hours, use a sand core funnel to filter, and dry the filter cake at 20-30°C for 2 hours to obtain carbetocin crude product II .

[0043] (3) Weigh 9.0g of carbetocin crude product II, add 270ml of 10% acetic acid solution, stir to dissolve, use reverse phase preparative high-performance liquid chromatography to purify, and collect carbetocin-containing elution for 25-35min. Fractions, the specific chromatographic conditions are as follows:

[0044] Equipment: Preparative HPLC, column diameter and length 60mm×300mm, packing C18

[0045] Mobile phase: A: 0.2% sodium acetate in water B: acetonitrile

[0046] Detection...

Embodiment 2

[0061] (1) Weigh 10.0 g of crude carbetocin, add it to 50 ml of methyl tert-butyl ether, beat at room temperature for 4 hours, use a sand core funnel to filter, and dry the filter cake at 20-30 ° C for 2 hours to obtain carbetocin Crude oxytocin I.

[0062] (2) Add the above-mentioned carbetocin crude product I to 50ml of 95% ethanol, beat at room temperature for 4 hours, use a sand core funnel to filter, and dry the filter cake at 20-30°C for 2 hours to obtain carbetocin crude product II .

[0063] (3) Weigh 9.0g of carbetocin crude product II, add 270ml of 10% acetic acid solution, stir to dissolve, use reverse phase preparative high-performance liquid chromatography to purify, and collect carbetocin-containing elution for 25-35min. Fractions, the specific chromatographic conditions are as follows:

[0064] Equipment: Preparative HPLC, column diameter and length 60mm×300mm, packing C18

[0065] Mobile phase: A: 0.2% sodium acetate in water B: acetonitrile

[0066] Detect...

Embodiment 3

[0081] (1) Weigh 10.0 g of crude carbetocin, add it to 50 ml of methyl tert-butyl ether, beat at room temperature for 4 hours, use a sand core funnel to filter, and dry the filter cake at 20-30 ° C for 2 hours to obtain carbetocin Crude oxytocin I.

[0082] (2) Add the above-mentioned carbetocin crude product I to 50ml of 95% ethanol, beat at room temperature for 4 hours, use a sand core funnel to filter, and dry the filter cake at 20-30°C for 2 hours to obtain carbetocin crude product II .

[0083] (3) Weigh 9.0g of carbetocin crude product II, add 270ml of 10% acetic acid solution, stir to dissolve, use reverse phase preparative high-performance liquid chromatography to purify, and collect carbetocin-containing elution for 25-35min. Fractions, the specific chromatographic conditions are as follows:

[0084] Equipment: Preparative HPLC, column diameter and length 60mm×300mm, packing C18

[0085] Mobile phase: A: 0.2% sodium acetate in water B: acetonitrile

[0086] Detect...

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Abstract

The invention discloses a purifying and refining method of carbetocin. The method comprises the following steps: sequentially pulping a carbetocin crude product with methyl tert-butyl ether, carrying out suction filtration, and drying a filter cake; beating the beaten dried solid with ethanol, carrying out suction filtration, and drying a filter cake; dissolving the obtained filter cake with an acetic acid aqueous solution, purifying by adopting reversed-phase preparative high performance liquid chromatography, and collecting an elution fraction containing carbetocin; concentrating the obtained carbetocin-containing elution fraction, purifying again by adopting a reversed-phase preparative high performance liquid chromatography, and collecting the carbetocin-containing elution fraction; and concentrating the obtained carbetocin-containing elution fraction, and freeze-drying the concentrated carbetocin-containing elution fraction in a freeze dryer to obtain a carbetocin pure product. The high-purity carbetocin is obtained through specific solvent pulping, two-time purification preparation through reversed-phase preparation and high-performance liquid chromatography and the like.

Description

technical field [0001] The invention relates to the field of medicine purification and refining, in particular to a method for purifying and refining carbetocin. Background technique [0002] The puerpera will be affected by many factors during childbirth, especially the phenomenon of postpartum hemorrhage, which can easily lead to maternal death and threaten the life and health of the puerpera. In recent years, my country's medical industry has developed rapidly, and there are more and more cesarean delivery methods. Under the influence of abnormal pregnancy and high-risk factors in pregnancy, the postpartum hemorrhage rate of pregnant women is further increased, which is also important for the smooth delivery of women. caused a certain impact. In order to ensure the healthy delivery of parturients, it is necessary to adopt a variety of technical means to improve the postpartum hemorrhage status of parturients to reduce the rate of postpartum hemorrhage and improve the safe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/16C07K1/20C07K1/34C07K1/36
CPCC07K7/16
Inventor 袁建坡陶艳萍
Owner CISEN PHARMA
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