Method for determining cvortioxetine intermediate and its isomers by using liquid chromatography

A technology of isomers and determination methods, which is applied in the directions of measuring devices, material separation, and analysis materials, etc., can solve problems such as incomplete removal of isomers, side reactions, and influence on drug purity and quality, and achieve improvement Yield and purity, reduced side reactions, quality-controlled effects

Inactive Publication Date: 2020-03-10
万全万特制药(厦门)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The incomplete removal of the isomers in the vortioxetine hydrobromide intermediate will cause side reactions and impurities in subsequent reactions, which will ultimately affect the purity and quality of the drug

Method used

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  • Method for determining cvortioxetine intermediate and its isomers by using liquid chromatography
  • Method for determining cvortioxetine intermediate and its isomers by using liquid chromatography
  • Method for determining cvortioxetine intermediate and its isomers by using liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Instruments and Conditions

[0038] LC-20AT pump, SPD-M20A detector, SIL-20AC autosampler, CBM-20A controller, CTO-10ASVP column thermostat, LC solution workstation

[0039] Chromatographic column: Welch (Ultimate PFP, 250×4.6mm, 5μm)

[0040] Mobile phase: A: 0.02mol / L dipotassium hydrogen phosphate buffer solution (adjust pH to 6.5 with phosphoric acid); B: methanol;

[0041] Elution was performed with the following gradient:

[0042]

[0043] Flow rate: 1.5mL / min

[0044] Detection wavelength: 220nm

[0045] Column temperature: 40°C

[0046] Injection volume: 10μL

[0047] Experimental procedure

[0048] Take an appropriate amount of vortioxetine hydrobromide intermediate and its isomers, dissolve the sample with methanol, and prepare each 1mL containing about 0.5 mg of vortioxetine hydrobromide intermediate and its isomers sample solution. Take an appropriate amount of the above-mentioned vortioxetine hydrobromide intermediate and its isomer solution to p...

Embodiment 2

[0050] Instruments and Conditions

[0051] High performance liquid chromatography: Shimadzu: LC-20AT pump, SPD-M20A detector, SIL-20AC autosampler, CBM-20A controller, CTO-10ASVP column thermostat, LC solution workstation

[0052] Chromatographic column: Kromasil (100-5PHENYL, 250×4.6mm, 5μm)

[0053] Mobile phase: A: 1% triethylamine aqueous solution (adjust pH to 6.5 with phosphoric acid), B: methanol;

[0054] T(min) 0 15 35 53 53.01 65 B% 25 30 60 60 25 25

[0055] Flow rate: 1.5mL / min

[0056] Detection wavelength: 220nm

[0057] Column temperature: 40°C

[0058] Injection volume: 10μL

[0059] Experimental procedure

[0060] Take an appropriate amount of vortioxetine hydrobromide intermediate and its isomers, dissolve the sample with methanol, and prepare each 1mL containing about 0.5 mg of vortioxetine hydrobromide intermediate and its isomers sample solution. Take an appropriate amount of the above-mentioned vortioxetine hydrobromi...

Embodiment 3

[0062] Instruments and Conditions

[0063] High performance liquid chromatography: Shimadzu: LC-20AT pump, SPD-M20A detector, SIL-20AC autosampler, CBM-20A controller, CTO-10ASVP column thermostat, LC solution workstation

[0064] Chromatographic column: Agilent (ZORBAX SB-Phenyl, 250×4.6mm, 5μm)

[0065] Mobile phase: A: 0.05mol / L potassium dihydrogen phosphate buffer solution (adjust the pH to 6.5 with potassium hydroxide); B: methanol;

[0066] T(min) 0 15 35 55 55.01 65 B% 30 35 70 70 30 30

[0067] Flow rate: 1.5mL / min

[0068] Detection wavelength: 220nm

[0069] Column temperature: 40°C

[0070] Injection volume: 10μL

[0071] Experimental procedure

[0072] Take an appropriate amount of vortioxetine hydrobromide intermediate and its isomers, dissolve the sample with methanol, and prepare respectively about 0.5 mg of each 1 mL of vortioxetine hydrobromide intermediate and its isomers. sample solution. Take an appropriate amount of t...

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Abstract

The invention belongs to the field of analytical chemistry. The invention discloses an analysis method for separating and determining a vortioxetine hydrobromide intermediate and its isomers by usingliquid chromatography. The method uses a chromatographic column filled with phenyl bonded silica gel as a filler and a certain proportion of a buffer salt solution-organic phase as a mobile phase, andcan quantitatively determinethe content of the vortioxetine hydrobromide intermediate and isomers thereof so that the mass of a vortioxetine hydrobromide starting material is effectively controlled,side reactions are reduced, and therefore it is guaranteed that the quality of a vortioxetine hydrobromide final product is controllable. The method is strong in specificity, high in accuracy and simple and convenient to operate.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring vortioxetine hydrobromide intermediate 2,4-dimethylthiophenol and its isomers by liquid chromatography. Background technique [0002] Vortioxetine hydrobromide is an antidepressant with multiple pharmacological activities, which is clinically used to treat major depressive disorder and generalized anxiety disorder. The English name of vortioxetine hydrobromide is VortioxetineHydrobromide, and its chemical name is 1-[2-(2,4-methylphenylthio)phenyl]piperazine hydrobromide (1-[2-(2,4 -dimethyl-phenylsulfanyl)phenyl]-piperazinehydrobromide), molecular formula is C 18 h 22 N 2 S. HBr. Vortioxetine hydrobromide intermediate chemical name is 2,4-dimethylthiophenol; molecular formula is C 8 h 10 S. Vortioxetine hydrobromide intermediate structural formula is: [0003] [0004] Isomer 1 I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/60
CPCG01N30/02G01N30/06G01N30/60G01N30/6052G01N2030/027G01N2030/062
Inventor 陈晓宇刘秋叶贾少华
Owner 万全万特制药(厦门)有限公司
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