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Purification method of carbetocin

A carbetocin, high-purity technology, applied in chemical instruments and methods, oxytocin/vasopressin, specific peptides, etc., can solve the problems of single separation method, low product purity, and low product yield. , to achieve the effect of reducing toxicity and cost

Inactive Publication Date: 2015-07-01
上海吉尔多肽有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a purification process suitable for large-scale industrial production of carbetocin, to solve the technical problems of single separation method, low product purity or low product yield in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1. Sample treatment: add a little acetonitrile to the carbetocin oxidation solution and sonicate until the liquid is clarified, filter through a filter membrane with a pore size of 0.45um, and collect the filtrate for later use.

[0018] 2. Purification

[0019] Purification conditions: Chromatographic column: a chromatographic column with octadecyl silica gel bonded silica gel as the stationary phase, the diameter and length of the column are: 5cm×25cm. Mobile phase: Phase A: 0.1% sodium perchlorate aqueous solution with a concentration of 0.1% by mass; Phase B: acetonitrile solution. Flow rate: 60-80ml / min. Detection wavelength: 220nm. Gradient: B% (mass percent concentration): 10-50%, 30-50min. The injection volume is 3.5-5g.

[0020] Purification process: equilibrate the chromatographic column with phase B with a concentration of 35% by mass, and then load the sample. The sample volume is 1.5-2.0L of sample solution. Linear gradient elution, collect the target ...

Embodiment 2

[0034] 1. Sample treatment: add a little acetonitrile to the carbetocin oxidation solution and sonicate until the liquid is clarified, filter through a filter membrane with a pore size of 0.45um, and collect the filtrate for later use.

[0035] 2. Purification

[0036] Purification conditions: Chromatographic column: a chromatographic column with octadecyl silica gel bonded silica gel as the stationary phase, the diameter and length of the column are: 10cm×25cm. Mobile phase: Phase A: 0.1% sodium perchlorate aqueous solution with a concentration of 0.1% by mass; Phase B: acetonitrile solution. Flow rate: 180-220ml / min. Detection wavelength: 220nm. Gradient: B% (mass percent concentration): 10-50%, 30-50min. The injection volume is 10-15g.

[0037] Purification process: equilibrate the chromatographic column with phase B with a mass percentage concentration of 35%, and then load the sample. The sample volume is 4-5L of sample solution. Linear gradient elution, collect the ...

Embodiment 3

[0051] 1. Sample treatment: add a little acetonitrile to the carbetocin oxidation solution and sonicate until the liquid is clarified, filter through a filter membrane with a pore size of 0.45um, and collect the filtrate for later use.

[0052] 2. Purification

[0053] Purification conditions: Chromatographic column: a chromatographic column with octadecyl silica gel bonded silica gel as the stationary phase, the diameter and length of the column are: 15cm×25cm. Mobile phase: Phase A: 0.1% sodium perchlorate aqueous solution with a concentration of 0.1% by mass; Phase B: acetonitrile solution. Flow rate: 650-850ml / min. Detection wavelength: 220nm. Gradient: B% (mass percent concentration): 10-50%, 30-50min. The injection volume is 15-20g.

[0054] Purification process: equilibrate the chromatographic column with phase B with a mass percentage concentration of 35%, and then load the sample. The sample volume is 8-10L of sample solution. Linear gradient elution, collect the...

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Abstract

The invention discloses a method for purifying carbetocin by virtue of a reversed-phase high-performance liquid chromatography. According to the method, the technical problems that separation methods are single, the product purity is low or the product yield is low by virtue of multiple measures in the prior art are solved. The method comprises the following steps: (1) filtering a carbetocin crude product solution by virtue of a 0.45-micron filter membrane for later use, carrying out gradient elution purification by virtue of a reverse phase silica gel column, and collecting a peptide solution with a target peak value, wherein a stationary phase of the reverse phase silica gel column is stearyl bonded silica gel, a mobile phase of the reverse phase silica gel column comprises a phase A and a phase B, the phase A is 0.1% sodium perchlorate, and the phase B is chromatographic grade acetonitrile; (2) converting the peptide solution into acetate by virtue of an ion exchange method; and (3) carrying out reduced pressure rotary evaporation concentration and freeze drying on the final high-purity peptide solution, so as to obtain powdery finished peptide. The method is applied to the industrial production of carbetocin.

Description

technical field [0001] The invention relates to the technical field of polypeptide reversed-phase HPLC, in particular to a method for batch industrial purification of carbetocin. Background technique [0002] Carbetocin is a synthetic long-acting nonapeptide analog of oxytocin with agonist properties. Like oxytocin, carbetocin binds to the oxytocin receptors of uterine smooth muscle, causing rhythmic contractions of the uterus, increasing its frequency and increasing uterine tension on the basis of the original contractions. It has no effect on the non-pregnant uterus, but has effective uterotonic effect on the pregnant uterus and the newly born uterus, and its clinical and pharmaceutical properties are similar to those of naturally occurring oxytocin. Oxytocin receptor levels in the uterus are low in the non-pregnant state, increase during pregnancy, and peak at parturition. [0003] After either intravenous or intramuscular injection of carbetocin, the uterus contracts r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/16C07K1/20
Inventor 徐红岩秦敬国杨翼
Owner 上海吉尔多肽有限公司
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