Analysis method for determining stereoisomers and intermediates in solifenacin succinate

A technology for solifenacin succinate and stereoisomers, which is applied in the field of analysis for the determination of stereoisomers and intermediates in solifenacin succinate, and can solve problems such as the detection of components not including two intermediates, and the like, Achieve the effect of improving testing methods, reducing testing costs and ensuring product quality

Active Publication Date: 2017-09-15
SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After searching, the separation method of related substances and stereoisomers of solifenacin succinate mentioned in ...

Method used

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  • Analysis method for determining stereoisomers and intermediates in solifenacin succinate
  • Analysis method for determining stereoisomers and intermediates in solifenacin succinate
  • Analysis method for determining stereoisomers and intermediates in solifenacin succinate

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Experimental program
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Effect test

Embodiment 1

[0051] Determination of Stereoisomers and Intermediates in Solinasine Succinate

[0052] (1) Instrument and chromatographic conditions

[0053] High performance liquid chromatography: Agilent 1260 high performance liquid chromatography system and workstation.

[0054] Chromatographic column: Amylose-tris(3,5-xylylcarbamate) bonded silica column (CHIRALPAKIA, 4.6mm×250mm, 5μm).

[0055] The mobile phase is n-hexane-anhydrous ethanol-isopropanol-diethylamine (80:10:10:0.1) (volume ratio), the flow rate is set to 1.0 mL / min, the detection wavelength is 220 nm, and the column temperature is 25°C.

[0056] (2) Experimental steps

[0057] Take a sample of solinacine succinate and an appropriate amount of impurity B, C, D, E, and F reference substances, and dissolve and dilute them with mobile phase to make each 1mL containing about 1mg of solinacine succinate and about 5μg of each impurity. Mix the solution as the test solution.

[0058] (3) Measurement methods and results

[0059] Take 10 μL o...

Embodiment 2

[0061] Determination of Stereoisomers and Intermediates in Solinasine Succinate

[0062] (1) Instrument and chromatographic conditions

[0063] High performance liquid chromatography: Agilent 1260 high performance liquid chromatography system and workstation.

[0064] Chromatographic column: Amylose-tris(3,5-xylylcarbamate) bonded silica column (CHIRALPAKIA, 4.6mm×250mm, 5μm).

[0065] The mobile phase is n-hexane-anhydrous ethanol-isopropanol-diethylamine (50:25:25:0.1) (volume ratio), the flow rate is set to 1.0 mL / min, the detection wavelength is 220 nm, and the column temperature is 25°C.

[0066] (2) Experimental steps

[0067] Take a sample of solinacine succinate and an appropriate amount of impurity B, C, D, E, and F reference substances, and dissolve and dilute them with mobile phase to prepare a sample containing about 1 mg of solinacine succinate and about 5 μg of each impurity in 1 mL Mix the solution as the test solution.

[0068] (3) Measurement methods and results

[0069] ...

Embodiment 3

[0071] Determination of Stereoisomers and Intermediates in Solinasine Succinate

[0072] (1) Instrument and chromatographic conditions

[0073] High performance liquid chromatograph: Agilent 1260 high performance liquid chromatography system and workstation.

[0074] Chromatographic column: Amylose-tris(3,5-xylylcarbamate) bonded silica gel column (CHIRALPAKIA, 4.6mm×250mm, 5μm).

[0075] The mobile phase is n-hexane-anhydrous ethanol-isopropanol-diethylamine (65:15:20:0.1) (volume ratio), the flow rate is set to 1.0 mL / min, the detection wavelength is 220 nm, and the column temperature is 20°C.

[0076] (2) Experimental steps

[0077] Take a sample of solinacine succinate and an appropriate amount of impurity B, C, D, E, and F reference substances, and dissolve and dilute them with mobile phase to prepare a sample containing about 1 mg of solinacine succinate and about 5 μg of each impurity in 1 mL Mix the solution as the test solution.

[0078] (3) Measurement methods and results

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Abstract

The invention relates to an analysis method for determining stereoisomers and intermediates in solifenacin succinate by adopting high-performance liquid chromatography. The analysis method is characterized in that high-performance liquid chromatography (HPLC) is adopted, and isocratic elution is carried out on an amylose-tris(3,5-dimethylphenyl carbamate) bonded silica gel chiral HPLC column; a mobile phase is n-hexane-absolute ethyl alcohol-isopropyl alcohol-diethylamine solution (65:15:20:0.1) (volume ratio); and the mobile phase is adopted to dissolve a sample. The method can be used for simultaneously determining enantiomers and a diastereoisomer of the solifenacin succinate and intermediates as mutual enantiomers, thus providing a more reliable guarantee for the research on new synthesis process routes for the solifenacin succinate and quality control.

Description

Technical field [0001] The invention relates to an analytical method for the determination of stereoisomers and intermediates in soline succinate, in particular to the enantiomers and diastereomers of soline succinate by high performance liquid chromatography A method for separation and quantitative determination of a conformer and two intermediates that are enantiomers of each other. Background technique [0002] The chemical name of Solinasine succinate is (3R)-1-azabicyclo[2,2,2]octan-3-yl(1S)-1-phenyl-3,4-dihydroisoquinoline- 2-(1H)-formate succinate is a highly selective bladder M receptor antagonist, and its main structure is Solinasine. [0003] [0004] There are two chiral centers in the new structure of Solina succinate and three optical isomers; the intermediate structure contains one chiral center and two optical isomers. According to the requirements of "Technical Guidelines for Impurity Research of Chemical Drugs", stereoisomers should be controlled as impurities in...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 孙玲于梦王金虎刘宪华郑天怡
Owner SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES
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