Method for separating and detecting optical isomer of brivaracetam starting material

A technique for optical isomers and gas chromatography, which is applied in the field of separation and determination of brivaracetam starting material and its optical isomers by gas chromatography, and can solve the problems of affecting the purity and quality of drugs, incomplete removal of optical impurities, etc. , to achieve the effect of ensuring purity and quality

Inactive Publication Date: 2020-03-10
万全万特制药(厦门)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Incomplete removal of optical impurities from the brivaracetam starting material will be introduced into the final API product, thereby affecting the purity and quality of the drug

Method used

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  • Method for separating and detecting optical isomer of brivaracetam starting material
  • Method for separating and detecting optical isomer of brivaracetam starting material
  • Method for separating and detecting optical isomer of brivaracetam starting material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Instruments and Conditions

[0037] Chromatograph: Agilent 6890 N gas chromatograph;

[0038] Detector: hydrogen flame ionization detector;

[0039] Chromatographic column: CYCLOSIL-B capillary column (Agilent, 30m×0.25mm*0.25μm)

[0040] Injection port temperature: 240°C;

[0041] Detector temperature: 280°C;

[0042] Carrier gas (nitrogen) flow rate: 1.0ml / min;

[0043] Split ratio: 20:1;

[0044] Injection volume: 1μl

[0045] Oven heating program:

[0046] Heating rate (℃ / min) temperature (°C) Hold time (min) / 60 0 20 160 0 5 180 3 5 220 8

[0047] Experimental procedure

[0048] Take an appropriate amount of the racemate of the starting material of brivaracetam, dissolve it with a solvent, and prepare a system suitability solution containing 1.0 mg / ml of the starting material of brivaracetam and its optical isomer; An appropriate amount of the starting material is dissolved in a solvent, prepared into a test soluti...

Embodiment 2

[0050] Chromatograph: Agilent 6890 N gas chromatograph;

[0051] Detector: hydrogen flame ionization detector;

[0052] Chromatographic column: CYCLOSIL-B capillary column (Agilent, 30m×0.25mm*0.25μm)

[0053] Injection port temperature: 240°C;

[0054] Detector temperature: 280°C;

[0055] Carrier gas (nitrogen) flow rate: 0.8ml / min;

[0056] Split ratio: 20:1;

[0057] Injection volume: 1μl

[0058] Oven heating program:

[0059] Heating rate (℃ / min) temperature (°C) Hold time (min) / 60 0 20 160 0 5 180 3 5 220 8

[0060] Experimental procedure

[0061]Take an appropriate amount of the racemate of the starting material of brivaracetam, dissolve it with a solvent, and prepare a system suitability solution containing 1.0 mg / ml of the starting material of brivaracetam and its optical isomers, inject it into a gas chromatograph, Analyze according to the above chromatographic conditions and record the chromatograms. see attached ...

Embodiment 3

[0063] Chromatograph: Agilent 6890 N gas chromatograph;

[0064] Detector: hydrogen flame ionization detector;

[0065] Chromatographic column: CYCLOSIL-B capillary column (Agilent, 30m×0.25mm*0.25μm)

[0066] Injection port temperature: 230°C;

[0067] Detector temperature: 250°C;

[0068] Carrier gas (nitrogen) flow rate: 1.0ml / min;

[0069] Split ratio: 20:1;

[0070] Injection volume: 1μl

[0071] Oven heating program:

[0072] Heating rate (℃ / min) temperature (°C) Hold time (min) / 60 0 20 160 0 5 180 3 5 220 8

[0073] Experimental procedure

[0074] Take an appropriate amount of the racemate of the starting material of brivaracetam, dissolve it with a solvent, and prepare a system suitability solution containing 1.0 mg / ml of the starting material of brivaracetam and its optical isomers, inject it into a gas chromatograph, Analyze according to the above chromatographic conditions and record the chromatograms. see attached...

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PUM

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Abstract

The invention belongs to the field of analytical chemistry. The invention discloses a method for rapidly separating and detecting the optical purity of a brivaracetam starting material (R)-4-propyl-dihydrofuran-2-one by using gas chromatography. According to the method, a cyclodextrin chiral capillary chromatographic column and a hydrogen flame ionization detector are adopted, so that the opticalpurity and the isomer content of the brivaracetam starting material can be quantitatively determined, and the stability of the optical isomer of the brivaracetam starting material is indicated. The method disclosed by the invention is strong in specificity, high in accuracy, good in durability and simple and rapid to operate.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring brivaracetam starting materials and optical isomers thereof by gas chromatography. Background technique [0002] Brivaracetam, an antiepileptic drug developed by UCB, has a wide range of antiepileptic activities and high safety. Epilepsy effect, for adjuvant treatment of partial seizures in epileptic patients over 16 years old. UCB submitted a new drug application to the US Food and Drug Administration (FDA) in 2015, and submitted a new drug application and marketing authorization application to the European Medicines Agency (EMA) and has been approved. According to the clinical research data of the original research company, Bowa The anticonvulsant ability of racetam is 10 times stronger than that of levetiracetam, the first brand drug in the field of epilepsy drugs, and it is expected to become a new leader in the epilepsy d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/60
CPCG01N30/02G01N30/06G01N30/60G01N30/6052G01N30/6078G01N2030/027G01N2030/062
Inventor 赵璐璐刘秋叶王宇杰
Owner 万全万特制药(厦门)有限公司
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