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Method for separation and determination of vortioxetine hydrobromide intermediate related substances by liquid chromatography

A technology of vortioxetine hydrobromide and its determination method, which is applied in the field of analytical chemistry, can solve problems such as side reaction impurities, incomplete removal of impurities, and influence on drug purity and quality, so as to reduce side reactions and improve yield and purity , quality controllable effect

Inactive Publication Date: 2017-04-19
万全万特制药江苏有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Incomplete removal of impurities in vortioxetine hydrobromide intermediates will cause side reactions and generation of impurities, which will ultimately affect the purity and quality of the drug

Method used

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  • Method for separation and determination of vortioxetine hydrobromide intermediate related substances by liquid chromatography
  • Method for separation and determination of vortioxetine hydrobromide intermediate related substances by liquid chromatography
  • Method for separation and determination of vortioxetine hydrobromide intermediate related substances by liquid chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Instruments and Conditions

[0036] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0037] Chromatographic column: C18 (Alltima, 250×4.6 mm, 5 μm);

[0038] Mobile phase: water: methanol-25:75;

[0039] Flow rate: 1.0mL / min;

[0040] Detection wavelength: 230nm;

[0041] Injection volume: 10μL;

[0042] Running time: 25min.

[0043] Experimental procedure

[0044] Take an appropriate amount of vortioxetine hydrobromide intermediate and its related substances, dissolve the sample with methanol, and prepare a sample solution containing about 1.0 mg / mL of vortioxetine hydrobromide intermediate and its related substances. Perform HPLC analysis according to the above conditions, and record the chromatograms. see attached results Figure 1~2 , figure 1 The chromatographic peak whose retention time is 18.106min is the vortioxetine hydrobromide intermediate, and all the other chromatographic peaks are the chromatog...

Embodiment 2

[0046] Instruments and Conditions

[0047] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0048] Chromatographic column: C18 (Alltima, 250×4.6 mm, 5 μm);

[0049] Mobile phase: water: methanol-30:70;

[0050] Flow rate: 1.0mL / min;

[0051] Detection wavelength: 230nm;

[0052] Injection volume: 10μL;

[0053] Running time: 40min.

[0054] Experimental procedure

[0055] Take an appropriate amount of vortioxetine hydrobromide intermediate and its related substances, dissolve the sample with methanol, and prepare a sample solution containing about 1.0 mg / mL of vortioxetine hydrobromide intermediate and its related substances. Perform HPLC analysis according to the above conditions, and record the chromatograms. see attached results Figure 3~4 , image 3 The chromatographic peak whose retention time is 27.112min is the vortioxetine hydrobromide intermediate, and all the other chromatographic peaks are the chromatogr...

Embodiment 3

[0057] Instruments and Conditions

[0058] High performance liquid chromatography: Shimadzu: LC-20AT, CBM-20A, SIL-20AC, SPD-M20A, CTO-10ASvp;

[0059] Chromatographic column: C18 (Alltima, 250×4.6 mm, 5 μm);

[0060] Mobile phase: A: water, B: methanol; elution is carried out according to the following gradient:

[0061] T(min) 0 8 35 35.01 45 B% 65 65 90 65 65

[0062] Flow rate: 1.0mL / min;

[0063] Detection wavelength: 230nm;

[0064] Injection volume: 10 μL.

[0065] Experimental procedure

[0066]Take an appropriate amount of vortioxetine hydrobromide intermediate and its related substances, dissolve the sample with methanol, and prepare a sample solution containing about 1.0 mg / mL of vortioxetine hydrobromide intermediate and its related substances; another appropriate amount of methanol as blank solvent. Perform HPLC analysis according to the above conditions, and record the chromatograms. see attached results Figure 5~7 , Figure ...

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Abstract

The invention belongs to the field of analytical chemistry, discloses a method for separation and determination of vortioxetine hydrobromide intermediate 1-bromo-2-iodo-benzene related substances by liquid chromatography. The method takes a chromatographic column with octadecylsilane bonded silica gel as a packing, takes a certain ratio of water-organic phase as a mobile phase, and can be used for quantitative determination of the contents of a vortioxetine hydrobromide intermediate and the related substances thereof, so as to effectively control the quality of the vortioxetine hydrobromide intermediate and ensure controllable quality of a vinpocetine hydrobromide final product. The method has the advantages of strong specificity, high accuracy and convenience in operation.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for separating and measuring vortioxetine hydrobromide intermediates and related substances by liquid chromatography. Background technique [0002] Vortioxetine hydrobromide can inhibit the reuptake of serotonin, and has the functions of 5-HT1A receptor agonist, 5-HT1B receptor partial agonist and 5-HT3', 5-HT1D and 5-HT7 receptor antagonist. For the treatment of major depressive disorder. The chemical name of the vortioxetine hydrobromide intermediate is 1-Bromo-2-iodo-benzene, and the molecular formula is C 6 h 4 BrI, the structural formula of vortioxetine hydrobromide intermediate is: [0003] . [0004] In the synthetic process of vortioxetine hydrobromide, it is necessary to control the purity of some key intermediates to reduce the occurrence of side reactions and the generation of impurities, thereby improving the yield and purity of the final product. T...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 曹祎宁王宇杰
Owner 万全万特制药江苏有限公司
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