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Analysis method of vernakalant related substances

An analysis method and technology related to substances, applied in the field of chemical analysis, can solve the problems of relatively large and difficult detection and separation, achieve optimal separation and improve the effect of symmetry

Pending Publication Date: 2022-03-18
SHANGHAI XUDONG HAIPU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Vernakalant intermediate A4 is shown in formula (III), because it contains a chiral center, there are multiple enantiomers, and one of the optical isomers is shown in formula (IV), because the structure is similar, Difficulty in detection and separation

Method used

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  • Analysis method of vernakalant related substances
  • Analysis method of vernakalant related substances
  • Analysis method of vernakalant related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Instruments and conditions: Waters e2695 high performance liquid chromatography

[0053] Chromatographic column: cellulose-tris((3,5-dichlorophenylcarbamate) chiral column DAICEL 4.6mm×250mm, 3μm);

[0054] Mobile phase volume ratio: the ratio of n-hexane-absolute ethanol-trifluoroacetic acid is 86:14:0.1;

[0055] Detection wavelength: 210nm;

[0056] Column temperature 30°C;

[0057] Flow rate: 1.0ml / min;

[0058] Injection volume: 10 μl.

[0059] Experimental steps:

[0060] Vernakalant intermediate A4: Accurately weigh an appropriate amount of Vernakalant intermediate A4 reference substance, dissolve it with the mobile phase, dilute it with the mobile phase to a solution containing about 2 μg per 1 ml, accurately measure 10 μl and inject it into the chromatograph, record Chromatogram, Vernakalant intermediate A4 chromatogram see figure 1 , the peak was at 17.098min.

[0061] Vernakalant intermediate A4 enantiomer: Accurately weigh an appropriate amount of t...

Embodiment 2

[0064] Instruments and conditions: Waters e2695 high performance liquid chromatography

[0065] Chromatographic column: cellulose-tris((3,5-dichlorophenylcarbamate) chiral column DAICEL 4.6mm×250mm, 3μm);

[0066] Mobile phase volume ratio: the ratio of n-hexane-absolute ethanol-trifluoroacetic acid is 85:15:0.1;

[0067] Detection wavelength: 210nm;

[0068] Column temperature 30°C;

[0069] Flow rate: 1.0ml / min;

[0070] Injection volume: 10 μl.

[0071] Test steps and results:

[0072] Precisely measure 10 μl of the test solution, inject it into the liquid chromatograph, record the chromatogram, see Figure 4 , the elution times of vernakalant intermediate A4 and its isomers were 15.571 min and 14.155 min, respectively, the separation degree of the two was 3.0, and the symmetry was good. Vernakalant intermediate A4 and its enantiomers were completely separated under these chromatographic conditions.

Embodiment 3

[0074] Instruments and conditions: Waters e2695 high performance liquid chromatography

[0075] Chromatographic column: cellulose-tris((3,5-dichlorophenylcarbamate) chiral column DAICEL 4.6mm×250mm, 3μm);

[0076] Mobile phase volume ratio: the ratio of n-hexane-absolute ethanol-trifluoroacetic acid is 95:5:0.1;

[0077] Detection wavelength: 210nm;

[0078] Column temperature 30°C;

[0079] Flow rate: 1.0ml / min;

[0080] Injection volume: 10 μl.

[0081] Test steps and results:

[0082] Precisely measure 10 μl of the test solution, inject it into the liquid chromatograph, record the chromatogram, see Figure 5 , the elution times of vernakalant intermediate A4 and its isomers were 44.211min and 36.910min respectively, the separation degree of the two was 5.7, and the symmetry was good. Vernakalant intermediate A4 and its enantiomers were completely separated under these chromatographic conditions.

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Abstract

The invention discloses a method for separating, analyzing and determining enantiomers of a vernakalant hydrochloride intermediate, which comprises the following steps: selecting a chiral stationary phase with cellulose-tri-(3, 5-dichlorophenyl carbamate) covalently bonded on the surface of silica gel as a filler, and taking a mixed solvent of n-hexane, absolute ethyl alcohol and trifluoroacetic acid in a certain proportion as a mobile phase; the method is used for separating and analyzing the enantiomer of the vernakalant hydrochloride intermediate A4.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography method, in particular to a chiral resolution method for resolving enantiomers of vernakalant hydrochloride intermediates, and the invention belongs to the field of chemical analysis. Background technique [0002] Vernakalant hydrochloride, [CAS: 748810-28-8 chemical name (3R)-1-[(1R,2R)-2-[2-(3,4-dimethoxyphenyl) )ethoxy] cyclohexyl] -3-pyrrolidinol hydrochloride], the chemical structural formula is as follows: [0003] [0004] Vernakalant is a novel atrial-selective class III antiarrhythmic drug. Jointly developed by Cardionme Pharma Pharmaceutical Company of Canada and Astellas Pharma Pharmaceutical Company of the United States, the mechanism of action is to selectively block the sodium and potassium (IKur) ion channels of the atria during the onset of atrial fibrillation, and inhibiting the IKur current can prolong the action potential duration of the atria , reduce the risk of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/32G01N30/54
CPCG01N30/02G01N30/06G01N30/34G01N30/32G01N30/54G01N2030/324
Inventor 杨易可周洁康文瑞梁屹
Owner SHANGHAI XUDONG HAIPU PHARMA
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