Purification method of oxytocin

A purification method, the technology of oxytocin, applied in the chemical industry, can solve the problems of unfavorable large-scale production process, environmental pollution, and residue, etc., and achieve the effects of low toxicity, reduced production cost, and high recovery rate

Inactive Publication Date: 2017-06-13
BENGBU BBCA MEDICINE SCI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Secondly, methanol and acetonitrile are used as solvents in this method. Methanol and acetonitrile are second-class solvents, which have certain toxicity and will remain in the final product, bringing a certain degree of risk to the application of the product. Therefore, the use of them should be restricted in the process. above solvent
In addition, the method of directly volatilizing the organic solvent in this process is firstly not conducive to the large-scale production process, and secondly, if this method is used, the direct volatilization of the organic solvent will cause great pollution to the environment

Method used

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  • Purification method of oxytocin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The refining purification method (1) of embodiment 1 oxytocin

[0025] 1. Concentration

[0026] Take 1 kg of oxytocin solution (2% by mass) and distill under reduced pressure at 45°C to 20% by mass, with a volume of 90ml.

[0027] 2. Crystallization

[0028] Add 90ml of the concentrated solution prepared in the first step to 120ml of ethanol, stir for 30min at 25-30°C, keep stirring in an ice bath at a temperature of -5-0°C for 18h, and a large amount of solids precipitate out.

[0029] 3. Filter and dry

[0030] After filtration, the solid was washed with 15 ml of ethanol, and the obtained solid was vacuum-dried at 40° C. for 5 hours to obtain 18.8 g of the product, with a total yield of 94%. The purity of the purified oxytocin was determined to be 97.01% by HPLC.

Embodiment 2

[0031] The refining purification method (2) of embodiment 2 oxytocin

[0032] 1. Concentration

[0033] Take 1 kg of oxytocin solution (2% by mass percentage) and distill it under reduced pressure at 40-45° C. to 20% by mass, with a volume of 90 ml.

[0034] 2. Crystallization

[0035] Add 90ml of the concentrated solution prepared in the first step to 90ml of isopropanol, stir for 30min at 25-30°C, keep stirring in an ice bath at a temperature of -10-0°C for 18h, and a large amount of solids precipitate out.

[0036] 3. Filter and dry

[0037] After filtering, the solid was washed with 15 ml of isopropanol, and the obtained solid was vacuum-dried at 45°C for 5 hours to obtain 15.42 g of the product, with a total yield of 77.1%. The content of purified oxytocin was 96.2% as determined by HPLC.

Embodiment 3

[0038] The refining purification method (3) of embodiment 3 oxytocin

[0039] 1. Concentration

[0040] Take 1kg of oxytocin solution (2% by mass) and distill it under reduced pressure at 40-45°C to 24% by mass, with a volume of 84ml.

[0041] 2. Crystallization

[0042] Add 84ml of the concentrated solution prepared in the first step to 90ml of isopropanol, stir for 30min at 25-30°C, keep stirring in an ice bath at a temperature of -10-0°C for 18h, and a large amount of solids precipitate out.

[0043] 3. Filter and dry

[0044] After filtering, the solid was washed with 15 ml of isopropanol, and the obtained solid was vacuum-dried at 45° C. for 5 hours to obtain 14.8 g of the product, with a total yield of 74%. HPLC content 96.4%.

[0045] It can be seen from the above examples that the process of the present invention is suitable for synthesis under laboratory conditions, the reaction raw materials and solvents are easy to get, there are no harsh reaction conditions, th...

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Abstract

The invention discloses a purification method of oxytocin, relating to the technical field of pharmaceutical synthesis and purification. The method comprises the following steps: by using an oxytocin water solution prepared by a chemical synthesis process as a raw material, concentrating the oxytocin water solution, adding an organic solvent for dissolution, cooling to crystallize, filtering and drying, thereby achieving the goal of purifying and refining the oxytocin. The method is simple to operate, lowers the production cost, and enhances the production efficiency of the enterprise. The prepared oxytocin has high purity. The method uses the single organic solvent, so the organic solvent has low toxicity, can be easily recovered and reutilized, and has small influence on the environment. Thus, the method is suitable for industrialized application.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for purifying oxytocin. Background technique [0002] Oxytocin, also known as oxytocin, is a nonapeptide compound composed of 8 amino acids containing a disulfide bond. Oxytocin is one of the main components of pituitary hormone in mammals and humans, and it is also a commonly used gynecological drug. It is mainly used clinically for induction of labor, postpartum hemorrhage, poor uterine reduction, and promotion of milk discharge. In the past, the production of oxytocin was mainly carried out through the tissue extraction of pig and bovine pituitary glands. At present, with the development of peptide chemical synthesis methods, it is mainly carried out through chemical synthesis methods. Many times of group protection and deprotection in the synthesis method, and the addition of catalysts are easy to remain in the final product and difficult to remove. [0003] At pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/16C07K1/30
Inventor 郑爱陈昀张瑾林文龙李立标
Owner BENGBU BBCA MEDICINE SCI DEV
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