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Atosiban acetate impurities and preparation and detection methods

A technology of atosiban acetate and impurities, which is applied in the field of active polypeptide impurities and its preparation, and can solve problems such as toxic and side effects

Inactive Publication Date: 2016-09-21
HAINAN HERUI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, many process impurities and degradation impurities produced during the synthesis of peptides are very similar to the structure of the main component. If these impurities are not well controlled, they may cause serious side effects

Method used

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  • Atosiban acetate impurities and preparation and detection methods
  • Atosiban acetate impurities and preparation and detection methods
  • Atosiban acetate impurities and preparation and detection methods

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0101] [embodiment 1] the preparation of impurity A

[0102](1) Weigh 2 g of atosiban acetate finished product, dissolve it ultrasonically with 80 ml of high-purity water, add 20 ml of 30% hydrogen peroxide under stirring, and perform an oxidation reaction for 2 hours to obtain a solution of impurity A;

[0103] (2) The oxidized solution is filtered through a 0.45um filter membrane, and purified by a semi-preparative high-performance liquid chromatograph, and the used chromatographic column is C 18 Filler, (10um, 21mm×250mm); each loading volume is 10ml (0.2g), with acetonitrile as mobile phase A, 0.05% TFA / H 2 O is the mobile phase B, the detection wavelength is 220nm, keep 15% mobile phase A for 10min, and change the mobile phase A to 45% within 10min to 50min, collect the component for 36-39min, which is impurity A component, and concentrate at 40°C Acetonitrile was removed, then bottled and freeze-dried to obtain impurity A. The purity of impurity A determined by liquid ...

Embodiment 2

[0104] [embodiment 2] the preparation of impurity A

[0105] (1) Weigh 2 g of atosiban acetate finished product, dissolve it ultrasonically with 80 ml of high-purity water, add 10 ml of 30% hydrogen peroxide under stirring, and perform an oxidation reaction for 1 hour to obtain a solution of impurity A;

[0106] (2) The oxidized solution is filtered through a 0.45um filter membrane, and purified by a semi-preparative high-performance liquid chromatograph, and the used chromatographic column is C 18 Filler, (10um, 21mm×250mm); each loading volume is 10ml (0.2g), with acetonitrile as mobile phase A, 0.05% TFA / H 2 O is the mobile phase B, the detection wavelength is 220nm, keep 15% mobile phase A for 10min, and change the mobile phase A to 45% within 10min to 50min, collect the component for 36-39min, which is impurity A component, and concentrate at 35°C Acetonitrile was removed, then bottled and freeze-dried to obtain impurity A. The purity of impurity A is 99.8% as determine...

Embodiment 3

[0107] [embodiment 3] the preparation of impurity A

[0108] (1) Weigh 2 g of atosiban acetate finished product, dissolve it ultrasonically with 80 ml of high-purity water, add 30 ml of 30% hydrogen peroxide under stirring, and perform an oxidation reaction for 3 hours to obtain a solution of impurity A;

[0109] (2) The oxidized solution is filtered through a 0.45um filter membrane, and purified by a semi-preparative high-performance liquid chromatograph, and the used chromatographic column is C 18 Filler, (10um, 21mm×250mm); each loading volume is 10ml (0.2g), with acetonitrile as mobile phase A, 0.05% TFA / H 2 O is the mobile phase B, the detection wavelength is 220nm, keep 15% mobile phase A for 10min, and change the mobile phase A to 45% within 10min to 50min, collect the component for 36-39min, which is impurity A component, and concentrate at 45°C Acetonitrile was removed, then bottled and freeze-dried to obtain impurity A. The purity of impurity A is 99.8% as determin...

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Abstract

The invention relates to atosiban acetate impurities and preparation and detection methods. The impurities are an impurity A or an impurity B or an impurity C or an impurity D or an impurity E, the sequence of the impurity A is c[Mpa(S=O)-D-Try(Et)Ile-Thr-Asn-Cys]-Pro-Orn-Gly-NH2, the sequence of the impurity B is c[Mpa-D-Tyr(Et)-Ile-Thr-Asn-Cys(S=O)]-Pro-Orn-Gly-NN2, the sequence of the impurity C is c[Mpa-D-Tyr(Et)-Ile-Thr-D-Asn-Cys]-Pro-Orn-Gly-NH2, the sequence of the impurity D is c[Mpa-D-Tyr(Et)-Ile-Thr-Asp-Cys]-Pro-Orn-Gly-NH2, and the sequence of the impurity E is c[Mpa-D-Tyr(Et)-Ile-Thr-Asn-Cys]-Pro-Orn-Gly-OH. The impurity A or the impurity B or the impurity C or the impurity D or the impurity E can serve as reliable contrast of process impurities produced in the atosiban acetate synthetic process or degradation impurities and can be used for qualitative and quantitative analysis of the impurities in atosiban acetate synthesis, and a way for further controlling the quality of atosiban acetate is opened.

Description

technical field [0001] The invention relates to an active polypeptide impurity and a preparation method thereof, in particular to an atosiban acetate impurity, a preparation and a detection method. Background technique [0002] Atosiban, English name: Atosiban, Atosiban is a nonapeptide, the peptide chain contains three unnatural amino acids D-Tyr (Et), Mpa and Orn and a pair of rings between Mpa and Cys Disulfide bond, its structural formula is: [0003] c[Mpa-D-Tyr(Et)-Ile-Thr-Asn-Cys]-Pro-Orn-Gly-NH 2 . [0004] Atosiban is a drug that can directly compete with oxytocin for oxytocin receptors and inhibit the combination of oxytocin and oxytocin receptors, thereby directly inhibiting the action of oxytocin on the uterus and inhibiting uterine contraction; it can also inhibit the hydrolysis of phosphatidylinositol role, blocking the production of second messengers and Ca 2+ activity, thereby indirectly inhibiting the uterine response to oxytocin and inhibiting uterine c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/16C07K7/06C07K1/36C07K1/30C07K1/20C07K1/06C07K1/04G01N33/68
CPCC07K7/16C07K7/06G01N33/6848G01N2410/04
Inventor 钟正明彭涛王玲
Owner HAINAN HERUI PHARMA
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