Semaglutide purifying method

A purification method and technology of samoglutide, which can be applied in the field of medicinal chemistry and can solve the problems of low yield and the like

Active Publication Date: 2016-07-20
HYBIO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the yield of the purification method of samaglutide in the prior art is low, resulting in the purification of samaglutide becoming a difficulty in the preparation process of samaglutide and one of the bottlenecks in the industrialization of samaglutide

Method used

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Examples

Experimental program
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Embodiment 1

[0064] Embodiment 1: Purification of samaglutide crude peptide

[0065] Source of experimental materials: Chromatographic column brand Kromasil; ammonium bicarbonate was purchased from Sinopharm Chemical Reagent Co., Ltd.; tetramethylammonium hydroxide was purchased from Aladdin; sodium dihydrogen phosphate was purchased from Sinopharm Chemical Reagent Co., Ltd.; ammonia water was purchased from Guangdong Guanghua Technology Co., Ltd.; glacial acetic acid was purchased from Guangdong Guanghua Technology Co., Ltd.

[0066] Butyl bonded silica column: Kromasil- -C4-10μm;

[0067] The source of the crude samaglutide peptide (that is, the sample of samaglutide to be purified): the company synthesizes it by itself.

[0068] The synthesis method is specifically:

[0069] Use Fmoc-Gly-King resin as the starting resin, add it to the solid-phase reaction column, wash 2 times with DMF, swell the Fmoc-Gly-King resin with DMF for 30 minutes, remove Fmoc protection with DBLK, and then ...

Embodiment 2

[0084] Example 2: Purification of Crude Peptide of Samoglutide

[0085] Source of experimental materials: chromatographic column brand Kromasil; potassium bicarbonate was purchased from Sinopharm Chemical Reagent Co., Ltd.; tetramethylammonium hydroxide was purchased from Aladdin; potassium dihydrogen phosphate was purchased from Sinopharm Chemical Reagent Co., Ltd.; ammonia water was purchased from Guangdong Guanghua Technology Co., Ltd.; glacial acetic acid was purchased from Guangdong Guanghua Technology Co., Ltd.

[0086] Butyl bonded silica column: Kromasil- -C4-10μm;

[0087] The source of samaglutide crude peptide (i.e. the samaglutide sample to be purified): same as Example 1, wherein the content of samaglutide is 52%.

[0088] Dissolve 2.0 g of crude samaglutide in a mixed solution of acetonitrile, water, and ammonia water (volume ratio of acetonitrile, ammonia water, and water = 15:5:80), filter, and collect the filtrate for later use.

[0089] 1. The first step:...

Embodiment 3

[0097] Example 3: Purification of Crude Peptide of Samoglutide

[0098] Source of experimental materials: Chromatographic column brand Kromasil; ammonium carbonate was purchased from Sinopharm Chemical Reagent Co., Ltd.; tetramethylammonium hydroxide was purchased from Aladdin; potassium dihydrogen phosphate was purchased from Sinopharm Chemical Reagent Co., Ltd.; ammonia water was purchased from Guangdong Guanghua Technology Co., Ltd.; Glacial acetic acid was purchased from Guangdong Guanghua Technology Co., Ltd.

[0099] Butyl bonded silica column: Kromasil- -C4-10μm;

[0100] The source of samaglutide crude peptide (i.e. the samaglutide sample to be purified): same as Example 1, wherein the content of samaglutide is 52%.

[0101] Dissolve 2.0 g of crude samaglutide peptide, filter, and collect the filtrate for later use.

[0102] 1. The first step: the first separation

[0103] Purification conditions: chromatographic column: a chromatographic column with butyl-bonded ...

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Abstract

The invention belongs to the technical field of pharmaceutical chemistry, and discloses a semaglutide purifying method. The purifying method comprises the following steps: taking a semaglutide sample to be purified, allowing the sample to go through a chemically bonded silica gel chromatographic column in order to carry out primary separation, carrying out gradient elution with an A1 solution and B solution mixed solution, and collecting an elution component to obtain a primary purification product; allowing the primary purification product to go through a chemically bonded silica gel chromatographic column in order to carry out secondary separation, carrying out gradient elution with an A2 solution and B solution mixed solution, and collecting an elution component to obtain a semaglutide solution, wherein the above A1 solution is a carbonate solution; the above A2 solution is a phosphate solution; and the B solution is an acetonitrile and isopropanol mixed solution with a volume ratio of acetonitrile to isopropanol of (8:2)-(9:1). The purifying method has the advantages of realization of high purity of the prepared semaglutide, substantial improvement of the semaglutide yield, simple operation, and facilitation of realization of large-scale preparation of semaglutide.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, in particular to a method for purifying samaglutide. Background technique [0002] Diabetes is a series of clinical syndromes caused by absolute or relative insufficiency of insulin in the body, which is closely related to genetics. The main clinical manifestations of diabetes are polydipsia, polyuria, polyphagia and weight loss, as well as high blood sugar and glucose in urine. There are four types of diabetes: type 1 diabetes, type 2 diabetes, other types of diabetes, and gestational diabetes. Any type of diabetes causes the beta cells in the pancreas to fail to produce enough insulin to lower blood sugar levels, resulting in hyperglycemia. According to the World Health Organization report in 2011, 346 million people worldwide suffer from diabetes. In 2004, an estimated 3.4 million people died from diseases caused by hyperglycemia. More than 80% of diabetes deaths occurred in low-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K14/00C07K1/16A61P3/10
Inventor 尹传龙康旭宓鹏程刘建马亚平袁建成
Owner HYBIO PHARMA
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