An analytical method for determining stereoisomers and intermediates in solifenacin succinate

A technology for solifenacin succinate and stereoisomers, which is applied in the field of analysis of stereoisomers and intermediates in solifenacin succinate, and can solve problems such as detection of two intermediate components not included, To achieve the effect of improving the detection method, reducing the detection cost and ensuring product quality

Active Publication Date: 2020-02-28
SHANDONG ACADEMY OF PHARMACEUTICAL SCIENCES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After searching, the separation method of related substances and stereoisomers of solifenacin succinate mentioned in the literature and patents did not include its 3 stereoisomers and 2 intermediate components that are enantiomers detection

Method used

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  • An analytical method for determining stereoisomers and intermediates in solifenacin succinate
  • An analytical method for determining stereoisomers and intermediates in solifenacin succinate
  • An analytical 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 Solifenacin 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 gel chromatographic column (CHIRALPAKIA, 4.6 mm×250 mm, 5 μm).

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

[0056] (2) Experimental steps

[0057] Take solifenacin succinate sample and appropriate amount of impurity B, C, D, E, F reference substance respectively, dissolve and dilute with mobile phase to make about 1 mg of solifenacin succinate and about 5 μg of each impurity in 1 mL The mixed solution was used as the test solution.

[0058] (3) Measurement method and res...

Embodiment 2

[0061] Determination of Stereoisomers and Intermediates in Solifenacin 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 gel chromatographic column (CHIRALPAKIA, 4.6 mm×250 mm, 5 μm).

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

[0066] (2) Experimental steps

[0067] Take solifenacin succinate sample and appropriate amount of impurity B, C, D, E, F reference substance respectively, dissolve and dilute with mobile phase to make about 1 mg of solifenacin succinate and about 5 μg of each impurity in 1 mL The mixed solution was used as the test solution.

[0068] (3) Measurement method and resu...

Embodiment 3

[0071] Determination of Stereoisomers and Intermediates in Solifenacin Succinate

[0072] (1) Instrument and chromatographic conditions

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

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

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

[0076] (2) Experimental steps

[0077] Take solifenacin succinate sample and appropriate amount of impurity B, C, D, E, F reference substance respectively, dissolve and dilute with mobile phase to make about 1 mg of solifenacin succinate and about 5 μg of each impurity in 1 mL The mixed solution was used as the test solution.

[0078] (3) Measurement method and res...

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Abstract

The invention relates to an analysis method for determining stereoisomers and intermediates in solifenacin succinate by using high performance liquid chromatography. It is characterized in that: high performance liquid chromatography is used to carry out isocratic elution on amylose-three (3,5-xylylcarbamate) bonded silica gel chiral chromatographic column; mobile phase is n-hexane- Absolute ethanol-isopropanol-diethylamine solution (65:15:20:0.1) (volume ratio); the sample is dissolved in mobile phase. This method can simultaneously determine the enantiomers, diastereomers and two intermediates of solifenacin succinate which are enantiomers, which is the research on the synthetic process route of solifenacin succinate And quality control to provide more reliable guarantee.

Description

technical field [0001] The invention relates to an analytical method for determining stereoisomers and intermediates in solifenacin succinate, in particular to the enantiomers and diastereoisomers of solifenacin succinate by high performance liquid chromatography. A method for the separation and quantitative determination of the enantiomer and two intermediates that are enantiomers. Background technique [0002] The chemical name of solifenacin succinate is (3R)-1-azabicyclo[2,2,2]octane-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 solifenacin. [0003] [0004] There are 2 chiral centers in the structure of solifenacin succinate, and there are 3 optical isomers; the structure of the intermediate contains 1 chiral center, and there are 2 optical isomers. According to the requirements of the "Technical Guiding Principles for Research on Impurities in Chemical Drugs", ste...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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