HPLC method for detecting cyclopropylamine in lenvatinib mesylate

A technology of lenvatinib mesylate and cyclopropylamine, which is applied in the field of HPLC analysis of cyclopropylamine, can solve the problems of inability to control the content of cyclopropylamine, low detection sensitivity, single product, etc., and achieves simple and easy analysis cost , single product, accurate and reliable results

Active Publication Date: 2020-06-09
SIMCERE ZAIMING PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since cyproamine has no ultraviolet absorption, gas-phase headspace method is often used for the determination of cyproamine, but lenvatinib mesylate is easily degraded to generate cyproamine under high temperature conditions, which interferes with detection, and a CAD detector is used for determination. The sensitivity is low, and the content of cyproamine in lenvatinib mesylate cannot be well controlled
[0003] There is no record in the prior art about the specific analytical method for detecting cyproamine from lenvatinib mesylate, and the HPLC pre-column derivatization method is used to measure cyproamine, which can avoid the interference of lenvatinib from high-temperature degradation and generation of cyproamine At the same time, the detection method has good resolution, the product after derivatization is single, and the blank has no interference peaks, which can accurately detect the content of cyclopropylamine in the sample

Method used

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  • HPLC method for detecting cyclopropylamine in lenvatinib mesylate
  • HPLC method for detecting cyclopropylamine in lenvatinib mesylate
  • HPLC method for detecting cyclopropylamine in lenvatinib mesylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take an appropriate amount of cyclopropylamine, add an appropriate amount of solvent [acetonitrile-water (80:20)], add a derivatization reagent 2,4-dinitrochlorobenzene solution to prepare a control solution, and use a diode array detector (DAD) to perform full-wavelength spectroscopy The results show that the maximum absorption of SCR-4341 derivatized chromatographic peaks is at 215nm, 264nm, and 356nm. At 356nm wavelength, the detection sensitivity is higher and the interference is less, so the 356nm wavelength is selected as the measurement wavelength of this product. See the detection spectrum figure 1 .

Embodiment 2

[0033] 1) Chromatographic conditions

[0034] Instrument: high performance liquid chromatography

[0035] Chromatographic column: Agilent Zorbax-Bonus-RP-C18 (150mm×4.6mm, 3.5μm)

[0036] Mobile phase: 0.05mol / L ammonium acetate solution (take 3.85g of ammonium acetate, add 1000ml of water to dissolve, add 1ml of glacial acetic acid to mix, adjust the pH to 5.0)-acetonitrile-methanol (18:11:11)

[0037] Solvent: acetonitrile - water (80:20)

[0038] Injection volume: 10μl

[0039] Detection wavelength: 356nm

[0040] 2) Sample preparation

[0041] (1) Accurately weigh an appropriate amount of SCR-4341 reference substance, prepare a solution containing about 7.5mg of SCR-4341 per 1ml, accurately measure 2ml into a 20ml headspace bottle, add lenvatinib mesylate 10mg, and accurately measure Take 0.5ml of sodium carbonate aqueous solution (take 2.5g of sodium carbonate, add 25ml of water to dissolve it) 0.5ml, add derivatization reagent 2,4-dinitrochlorobenzene solution (take...

Embodiment 3

[0048] 1) Chromatographic conditions

[0049] Instrument: high performance liquid chromatography

[0050] Chromatographic column: Agilent Zorbax-Bonus-RP-C18 (150mm×4.6mm, 3.5μm)

[0051] Mobile phase: 0.05mol / L ammonium acetate solution (take 3.85g of ammonium acetate, add 1000ml of water to dissolve, add 1ml of glacial acetic acid to mix, adjust the pH to 5.0)-acetonitrile-methanol (18:11:11)

[0052] Solvent: acetonitrile - water (80:20)

[0053] Injection volume: 10μl

[0054] Detection wavelength: 356nm

[0055] 2) Sample preparation

[0056] Accurately weigh an appropriate amount of cyproteramine reference substance, add solvent acetonitrile-water (80:20) and quantitatively dilute to make a solution containing about 7 μg per 1ml as the reference substance solution, take 2ml of the reference substance stock solution and put it in a 20ml headspace bottle, add derivative Chemical reagent 2,4-dinitrochlorobenzene solution (1mg / ml) 0.1ml or 1ml, investigate 40 ℃, 60 ℃ an...

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Abstract

The invention discloses an HPLC (High Performance Liquid Chromatography) method for detecting cyclopropylamine in lenvatinib mesylate, The method is characterized in that the method adopts a reversed-phase chromatographic column and uses derivatization reagent to perform derivatization treatment of a to-be-detected sample, and a mobile phase is selected from salt buffer solution containing amine substances and organic solvent. The method can be used for accurately detecting the content of cyclopropylamine in lenvatinib mesylate, is simple and feasible, is low in analysis cost, is accurate andreliable in result, and is convenient for controlling the product quality in the production and quality control process.

Description

technical field [0001] The present invention relates to the HPLC analysis method of cyclopropylamine. Background technique [0002] Cyclopropylamine (SCR-4341) is the starting material used in the third step of the synthesis reaction of lenvatinib mesylate. Since cyproamine has no ultraviolet absorption, gas-phase headspace method is often used for the determination of cyproamine, but lenvatinib mesylate is easily degraded to generate cyproamine under high temperature conditions, which interferes with the detection. In addition, a CAD detector is used for determination. The sensitivity is low, and the content of cyproamine in lenvatinib mesylate cannot be well controlled. [0003] There is no record in the prior art about the specific analytical method for detecting cyproamine from lenvatinib mesylate, and the HPLC pre-column derivatization method is used to measure cyproamine, which can avoid the interference of lenvatinib from high-temperature degradation and generation o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
CPCG01N30/89
Inventor 王霞梁春谊杨新华李薇任晋生
Owner SIMCERE ZAIMING PHARM CO LTD
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