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Method for detecting R-3-quinuclidinol in solifenacin succinate

A technology of solifenacin succinate and a detection method, which is applied in the field of quantitative analysis, can solve the problems of low detection sensitivity, accuracy, operation sensitivity, and inability to quantitative analysis of thin-layer chromatography, and achieves good detection effect and sensitivity. and high accuracy and reproducibility

Active Publication Date: 2016-04-20
迪嘉药业集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low detection sensitivity of thin-layer chromatography, quantitative analysis is not possible, and the color development time is long, its accuracy and operational sensitivity are not as good as those of high-performance liquid chromatography.

Method used

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  • Method for detecting R-3-quinuclidinol in solifenacin succinate
  • Method for detecting R-3-quinuclidinol in solifenacin succinate
  • Method for detecting R-3-quinuclidinol in solifenacin succinate

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Experimental program
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Effect test

Embodiment 1

[0024] Embodiment 1: the selection of mobile phase system

[0025] R -3-quinine alcohol positioning solution: precise weighing R - About 10mg of 3-quinine alcohol, put it in a 10ml measuring bottle, add mobile phase to dissolve and dilute to the mark, as R - 3-quinine alcohol positioning solution.

[0026] Solifenacin succinate positioning solution: Precisely weigh about 25 mg of solifenacin succinate raw material from Disa Pharmaceutical Group SLNX-07-63-34-15 batch, put it in a 50ml measuring bottle, dissolve and dilute the mobile phase to Scale, as solifenacin succinate positioning solution.

[0027] Mixed solution: precise weighing R -3-quinine alcohol and solifenacin succinate in appropriate amount, add mobile phase to dissolve and quantitatively dilute to make each 1ml contain about R - A solution of 1 mg of 3-quinine alcohol and 0.5 mg of solifenacin succinate as a mixed solution.

[0028] Determination conditions: choose IntersilNH2 (4.6×250mm, 5μm) chromatograph...

Embodiment 2

[0034] R -3-quinine alcohol reference substance solution: take R - The appropriate amount of 3-quinine alcohol, accurately weighed, add mobile phase to dissolve and quantitatively dilute to make about 1ml of R - 3-quinine alcohol 0.02 mg solution, as R -3-quinine alcohol reference substance solution.

[0035] The solution of the test product: Take the appropriate amount of solifenacin succinate raw material batch from Disha Pharmaceutical Group SLNX-07-63-34-15, accurately weigh it, add mobile phase to dissolve and dilute to make about succinic acid per 1ml Solifenacin 20mg solution, as the test substance.

[0036]Determination conditions: choose IntersilNH2 (4.6×250mm, 5μm) chromatographic column, Hitachi D-2000 high performance liquid chromatography, mobile phase: n-hexane-ethanol-methanol-diethylamine (600:300:100:1, v / v / v / v), the flow rate is 1.0ml / min, the column temperature is 30°C, the detector is an ultraviolet detector, the detection wavelength is 210nm, and the ...

Embodiment 3

[0038] Embodiment 3: method verification

[0039] (1) Precision precision weighing R - about 10mg of 3-quinine alcohol, put it in a 50ml measuring bottle, add mobile phase to dissolve and dilute to the mark, as R - 3-quinine alcohol stock solution; R - 1ml of 3-quinine alcohol stock solution was placed in a 10ml measuring bottle, and the mobile phase was diluted to the mark as a reference solution. The reference substance solution was continuously injected 6 times, and the RSDs of retention time and peak area were 0.12% and 0.47%, respectively, and the precision was good.

[0040] (2) Detection limit and quantification limit take the above R - 3-quinuclidinol stock solution, add mobile phase to gradually dilute and inject sample for detection, when the signal-to-noise ratio is about 3:1 and 10:1 respectively, the concentration is the detection limit and quantification limit of 3-quinuclidinol. The detection limit is 6.11μg / ml, which is equivalent to 0.03% of the concentrat...

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Abstract

The invention provides an analysis method for detecting R-3-quinuclidinol in solifenacin succinate by high performance liquid chromatography. The method is characterized in that high performance liquid chromatography is adopted, and a chromatographic column adopting aminopropyl bonded silica gel as a filling agent is employed; an ultraviolet detector which has the detection wavelength of 210 nm is used; the mobile phase is an n-hexane-ethanol-methanol-diethylamine (600:300:100:1) solution; a sample is dissolved by the mobile phase and has the concentration of 20 mg / ml, and quantitative analysis is made according to peak area by the external standard method. The method has the advantages of being good in selectivity, high in sensitivity and accuracy, excellent in repeatability, and simple, convenient and quick, and provides a guarantee for accurate detection of R-3-quinuclidinol in solifenacin succinate.

Description

technical field [0001] The present invention is a method of utilizing high performance liquid chromatography to detect solifenacin succinate R - New technology for 3-quinine alcohol, suitable for its quantitative analysis. Background technique [0002] Solifenacin succinate (solifenacin), chemical name (3 R )-1-azabicyclo-[2,2,2]octane-3-yl (1 S )-1-phenyl-3,4-dihydroisoquinoline-2 (1 H )-formate succinate, a muscarinic M3-receptor antagonist. It is used as a urethral antispasmodic to treat the symptoms of overactive bladder, and its structural formula is as attached figure 1 shown. Solifenacin succinate was launched in the Netherlands, Germany, the United Kingdom, France and Denmark in 2004, in the United States in 2005, and in China in 2009. So far, it has been marketed in more than 50 countries and regions around the world. [0003] The summary of clinical practice shows that the adverse reactions of drugs are not only related to the pharmacological activity of the ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 王西宁王东武丛日刚宋莹雪姜晓军
Owner 迪嘉药业集团股份有限公司
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