Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Liquid chromatographic method for separating and determining multiple impurities in tolvaptan

A technology of tolvaptan and high-performance liquid chromatography, applied in the field of drug analysis, to achieve the effects of improved safety, strong specificity, and accurate and reliable determination results

Active Publication Date: 2015-10-28
CHENGDU BAIYU PHARMA CO LTD
View PDF2 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are no relevant reports on the detection methods of the positional isomer impurities II, III of tolvaptan I and the positional isomer impurities V and VI of tolvaptan intermediate IV

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Liquid chromatographic method for separating and determining multiple impurities in tolvaptan
  • Liquid chromatographic method for separating and determining multiple impurities in tolvaptan
  • Liquid chromatographic method for separating and determining multiple impurities in tolvaptan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Embodiment 1 Detection condition of the present invention

[0061] High performance liquid chromatography: LC-20AT, SPD-20A

[0062] Column: Symmetry shield TM RP18 (4.6×150mm, 5μm);

[0063] Mobile phase: acetonitrile-water (containing 0.2% phosphoric acid) (45:55);

[0064] Flow rate: 1.0mL / min;

[0065] Detection wavelength: 254nm;

[0066] Column temperature: 25°C;

[0067] Injection volume: 10 μL.

[0068] Detection steps:

[0069] Take an appropriate amount of the reference substances of impurities II, III, IV, V and VI, dissolve them in methanol, and prepare a reference substance solution containing about 6.0 μg per 1 mL

[0070] Determination method: Take 10 μL of the above solution and inject it into the liquid chromatograph, record the chromatogram, the result is as follows: figure 1 shown. The chromatographic peak separation degree of impurity Ⅱ and impurity Ⅲ in the spectrum is 1.518; the chromatographic peak separation degree of impurity Ⅴ and imp...

Embodiment 2

[0119] Embodiment 2 Detection of tolvaptan and its impurities

[0120] Detection conditions:

[0121] High performance liquid chromatography: LC-20AT, SPD-20A

[0122] Column: Symmetry shield TM RP18 (4.6×150mm, 5μm);

[0123] Mobile phase: acetonitrile-water (containing 0.2% phosphoric acid) (45:55);

[0124] Flow rate: 1.0mL / min;

[0125] Detection wavelength: 254nm;

[0126] Column temperature: 25°C;

[0127] Solvent: Methanol;

[0128] Injection volume: 10 μL.

[0129] a, get tolvaptan I (crude product) 10mg, put in 10mL measuring bottle, add solvent to dissolve and dilute to scale, as need testing solution;

[0130] b. Take an appropriate amount of impurity II, III, IV, V and VI reference substances, dissolve and dilute them with solvents respectively to make reference substance solutions with a concentration of about 1.0 μg / mL;

[0131] C, get the need testing solution of step a and the reference substance solution of step b respectively, inject high performance ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Lengthaaaaaaaaaa
The inside diameter ofaaaaaaaaaa
Particle sizeaaaaaaaaaa
Login to View More

Abstract

The invention discloses a liquid chromatographic method for separating and determining multiple impurities in tolvaptan. High performance liquid chromatographic detection conditions are that detection wavelength is 230 to 280 nm, a chromatographic column is Symmetry shield RP18 and a mobile phase is acetonitrile-aqueous solution containing 0.2% phosphoric acid, wherein the volume fraction of acetonitrile is 43 to 47%. The method provided by the invention overcomes problems in separation and determination of tolvaptan and five impurities thereof, especially problems in separation and determination of positional isomer impurities of tolvaptan and positional isomer impurities of tolvaptan intermediates; and the method has the advantages of good specificity, simplicity, rapidness, accuracy and accurate and reliable determination results, so the quality of tolvaptan can be effectively monitored, and drug security is improved.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a liquid chromatography method for separating and measuring multiple impurities in tolvaptan. Background technique [0002] Tolvaptan (Tolvaptan trade name: Samsca), chemical name N-[4-[(5RS)-7-chloro-5-hydroxy-2,3,4,5-tetrahydro-1H-benzo[b ]azepine-1-formyl]-3-methylphenyl]-2-methylbenzamide (molecular weight: C 26 h 25 ClN 2 o 3 ), whose chemical structural formula is shown in formula I, is an oral selective non-peptide novel arginine vasopressin V2 receptor antagonist developed by Otsuka Pharm. The US FDA approved it in May 2009 for the treatment of hypercapacity or isovolumic hyponatremia (serum sodium < 125 mg) caused by congestive heart failure (CHF), liver cirrhosis, and antidiuretic hormone insufficiency syndrome. / L, or mild symptoms). Oral administration of tolvaptan tablets can significantly reduce the patient's body weight and edema without disrupting the blood e...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): G01N30/02
Inventor 夏玉立孙毅
Owner CHENGDU BAIYU PHARMA CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com