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High performance liquid chromatography method for lisinopramine dimesylate and intermediate impurities thereof

A kind of analytical method, the technology of dextroamphetamine, applied in analytical field, can solve the problems such as no relevant bibliographical reports

Active Publication Date: 2020-10-20
YICHANG HUMANWELL PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] At present, there is no relevant literature report on the analytical method for the simultaneous detection of lisdexamfetamine dimesylate and the above three intermediate impurities

Method used

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  • High performance liquid chromatography method for lisinopramine dimesylate and intermediate impurities thereof
  • High performance liquid chromatography method for lisinopramine dimesylate and intermediate impurities thereof
  • High performance liquid chromatography method for lisinopramine dimesylate and intermediate impurities thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Chromatographic conditions:

[0058] High performance liquid chromatograph: Dinoex U3000;

[0059] Chromatographic column: Welch Ultimate XB-C8 (150×4.6mm, 5μm);

[0060] Column temperature: 40℃;

[0061] Detection wavelength: 220nm;

[0062] Flow rate: 1.5ml / min;

[0063] Injection volume: 20 μl.

[0064] With 0.2v% triethylamine, 0.02M tetrabutylammonium hydrogen sulfate solution as mobile phase A, phosphoric acid to adjust pH to 7.0, acetonitrile as mobile phase B, gradient elution was performed, and the gradient elution conditions were:

[0065]

[0066]

[0067] Experimental steps:

[0068] Take an appropriate amount of lisdexamphetamine dimethanesulfonate and its intermediate impurities, dissolve the sample with methanol respectively, prepare a mixed solution containing about 0.3 mg / ml of lisdexamphetamine dimethanesulfonate and each intermediate, and take an appropriate amount of methanol as a blank solvent . Measure 20 μl of the above solution and i...

Embodiment 2

[0070] High performance liquid chromatograph: Dinoex U3000;

[0071] Chromatographic column: Waters XBridge-C8 (150×4.6mm, 5μm);

[0072] Column temperature: 40℃;

[0073] Detection wavelength: 220nm;

[0074] Flow rate: 1.5ml / min;

[0075] Injection volume: 20 μl.

[0076] Using 0.02M tetrabutylammonium hydrogen sulfate solution containing 0.2v% triethylamine as mobile phase A, adjusting the pH to 7.0 with phosphoric acid, and acetonitrile as mobile phase B, carry out gradient elution. The gradient elution conditions are:

[0077] time (min) Mobile phase A (V%) Mobile phase B (V%) 0 95 5 20 70 30 30 15 85 33 15 85 34 95 5 40 95 5

[0078] Experimental steps:

[0079] Get an appropriate amount of lisdexamphetamine dimethanesulfonate and its intermediate impurities, dissolve the sample with methanol respectively, prepare a mixed solution containing about 0.3 mg / ml of lisdexamphetamine dimethanesulfonate and each intermed...

Embodiment 3

[0081] High performance liquid chromatograph: Dinoex U3000;

[0082] Chromatographic column: Welch Ultimate XB-C8 (150×4.6mm, 5μm);

[0083] Column temperature: 40℃;

[0084] Detection wavelength: 220nm;

[0085] Flow rate: 1.5ml / min;

[0086] Injection volume: 20 μl.

[0087] Using 0.2v% triethylamine and 0.01M tetrabutylammonium hydrogen sulfate solution as mobile phase A, pH adjusted to 7.0 with phosphoric acid, and acetonitrile as mobile phase B, gradient elution was performed. The gradient elution conditions were:

[0088] time (min) Mobile phase A (V%) Mobile phase B (V%) 0 95 5 20 70 30 30 15 85 33 15 85 34 95 5 40 95 5

[0089] Experimental steps:

[0090] Get an appropriate amount of lisdexamphetamine dimethanesulfonate and its intermediate impurities, dissolve the sample with methanol respectively, prepare a mixed solution containing about 0.3 mg / ml of lisdexamphetamine dimethanesulfonate and each intermediate...

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Abstract

The invention discloses a high performance liquid chromatography method of lisinopramine dimesylate and intermediate impurities thereof. The method adopts an octyl silane bonded silica gel column as achromatographic column, a buffer solution as a mobile phase A and a polar organic solvent as a mobile phase B to carry out gradient elution. The method can be used for effectively analyzing lisinopiramine dimesylate and intermediate impurities thereof, and the separation degree between impurity peaks and between a main peak and an adjacent peak is good. The method is simple to operate and rapid in analysis, has good stability and specificity, and provides a simple and reliable analysis method for quality control of lisinophen dimesylate.

Description

technical field [0001] The invention belongs to, but is not limited to, the technical field of analysis, and specifically relates to, but is not limited to, a method for utilizing high performance liquid chromatography to analyze lisdexamphetamine dimesylate and intermediate impurities thereof. Background technique [0002] Lisdexamphetamine dimesylate, chemical name ((2S)-2,6-diamino-N-[(1S)-1-methyl-2-phenylethyl]hexanamide dimethanesulfonate) , molecular formula C 17 H 33 N 3 O 7 S 2 , the chemical structure is as follows. [0003] [0004] Patents WO2015130660A1, WO2015130660A1, WO2015130661A1, US2009234002A1, WO03072046A2, US2007042955A1, US2005054561A1, JP2012006978A and US201215706A1 disclose the synthesis route of dextromethansulfonic acid as shown below. [0005] [0006] [0007] In the process of synthesizing this compound, some important intermediates may be removed incompletely, and process impurities may be introduced, thereby affecting the quali...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027
Inventor 张巧银张丽娜汪淼田峦鸢陈怡郭建锋李莉娥李仕群吕金良杜文涛朱圣姬杨小青
Owner YICHANG HUMANWELL PHARMA
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