Preparation method of high-purity oxytocin

An oxytocin, high-purity technology, applied in the field of biomedicine, can solve the problems of low yield, low purity, difficult purification, etc., and achieve the effects of low impurity content, high yield and reducing adverse reactions

Active Publication Date: 2020-07-28
NANJING GRITPHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the technical problems of low yield, low purity and difficult purification in the prior art, the present invention provides a method for purifying oxytocin, which can obtain high-purity oxytocin with high yield

Method used

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  • Preparation method of high-purity oxytocin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Take 100g of crude oxytocin, add 70mL of water, and heat to 45°C to form a homogeneous solution. Add 35 mL of ethanol, slowly cool down to 15°C, let stand for 12 hours, filter, and wash the filter cake with ethanol to obtain the first batch of pure oxytocin.

[0034] (2) Add 20 mL of ethanol to the mother liquor in step (1), lower the temperature to 5° C., let it stand for 12 hours, and filter to obtain the primary pure oxytocin.

[0035] (3) The pure product of oxytocin was dissolved in 30mL of acetone, heated to 40°C, a small amount of solid oxytocin was added as a seed crystal, 5mL of acetone solvent was slowly volatilized, and then the temperature was slowly lowered to 5°C, the solid was precipitated, filtered by suction, and oxytocin was obtained. The second batch of Gongsu pure product.

[0036] (4) The first batch and the second batch of pure oxytocin were combined and freeze-dried to obtain 92.6 g of oxytocin raw material, and the content of related substan...

Embodiment 2

[0038] (1) Take 100g of crude oxytocin, add 70mL of water, and heat to 50°C to form a homogeneous solution. Add 40 mL of ethanol, slowly cool down to 20°C, let stand for 12 hours, filter, and wash the filter cake with ethanol to obtain the first batch of pure oxytocin.

[0039] (2) Add 25 mL of ethanol to the mother liquor in step (1), cool down to 0° C., let stand for 12 hours, and filter to obtain the primary pure oxytocin.

[0040] (3) The pure product of oxytocin was dissolved in 30mL of acetone, heated to 40°C, a small amount of solid oxytocin was added as a seed crystal, 6mL of acetone solvent was slowly volatilized, and then the temperature was slowly lowered to 5°C. The second batch of Gongsu pure product.

[0041] (4) The first batch and the second batch of pure oxytocin were combined and freeze-dried to obtain 91.2 g of oxytocin raw material, and the content of related substances was determined.

Embodiment 3

[0043] (1) Take 100g of crude oxytocin, add 70mL of water, and heat to 45°C to form a homogeneous solution. Add 35 mL of ethanol, slowly cool down to 15°C, let stand for 12 hours, filter, and wash the filter cake with ethanol to obtain the first batch of pure oxytocin.

[0044] (2) Add 25 mL of ethanol to the mother liquor in step (1), cool down to 0° C., let stand for 12 hours, and filter to obtain the primary pure oxytocin.

[0045] (3) The pure product of oxytocin was dissolved in 30mL of acetone, heated to 40°C, a small amount of solid oxytocin was added as a seed crystal, 4mL of acetone solvent was slowly volatilized, and then the temperature was slowly lowered to 5°C, the solid was precipitated, filtered by suction, and oxytocin was obtained. The second batch of Gongsu pure product.

[0046] (4) The first batch and the second batch of pure oxytocin were combined and freeze-dried to obtain 89.2 g of oxytocin raw material, and the content of related substances was determi...

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Abstract

The present invention belongs to the technical field of biomedicine and specifically relates to a preparation method of high-purity oxytocin. An oxytocin crude product is purified by grading and twicerecrystallization. The oxytocin crude product is dissolved in hot water, ethanol is added, cooling is conducted for crystallization and a first batch of pure oxytocin is obtained; ethanol is added tomother liquid again, cooling is conducted for crystallization and an oxytocin primary pure product is obtained; the oxytocin primary pure product is dissolved with acetone, a solvent is evaporated, at the same time, cooling is conducted for crystallization and a second batch of pure oxytocin is obtained. The method has a high production yield of the oxytocin, can also control impurity content of1% or less, and obtains an oxytocin raw material with low impurity content and good stability.

Description

technical field [0001] The invention belongs to the technical field of biomedicine. Specifically relates to a preparation method of high-purity oxytocin. Background technique [0002] Oxytocin (also known as oxytocin, oxytocin) is the first neuropeptide whose structure is determined, and the structure is shown in Formula 1. In 1909, Blair et al. reported the uterotonic effect of pituitary extracts from pregnant pigs. In 1910, Ott and Scott demonstrated the milk-ejecting effect of the extract. In 1949, oxytocin was isolated from this extract in a highly pure form. A few years later, deVigneaud et al determined the amino acid sequence of OT and first synthesized OT in 1954. This is the first time in human history that a biologically active peptide hormone has been successfully synthesized, which is of epoch-making significance. For this reason, de Vigneaud won the Nobel Prize in Chemistry in 1955. [0003] [0004] Oxytocin was originally extracted from the pituitary g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/16C07K1/30
CPCC07K7/16
Inventor 陆滢炎熊汝菊匡小录周静罗琦赵卿霍立茹李战
Owner NANJING GRITPHARMA CO LTD
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