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Apremilast related substance determination method

A determination method and related substance technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of insufficient research on synthesis process impurities and degradation products, complex mobile phase system, long analysis time, etc., to achieve high sensitivity, analytical The effect of short time and simple mobile phase system

Active Publication Date: 2021-10-22
JIANGSU SIMCERE PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing detection methods are insufficient for the research on the synthesis process impurities and degradation products of Apremilast, and the mobile phase system is relatively complex, the analysis time is long, and the sensitivity is low

Method used

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  • Apremilast related substance determination method
  • Apremilast related substance determination method
  • Apremilast related substance determination method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Instruments and Conditions

[0070] Agilent 1260 liquid chromatograph and chemical workstation; automatic sample injection; Agilent Eclipse PlusC18 column (150*4.6mm, 3.5μm) as separation column; UV detector wavelength: 210nm; mobile phase: 10mmol / L diphosphate Potassium hydrogen solution (adjust the pH value to 2.8 with phosphoric acid) is mobile phase A, acetonitrile is mobile phase B, gradient elution; 0 minutes to 3 minutes, mobile phase A is 90% (V / V), mobile phase B is 10% (V / V); 3 minutes to 25 minutes, mobile phase A linearly decreased to 45% (V / V), mobile phase B linearly increased to 55% (V / V); 25 minutes to 30 minutes, mobile phase A linearly decreased to 20% (V / V), mobile phase B linearly increased to 80% (V / V); 30 minutes to 40 minutes, mobile phase A was 20% (V / V), mobile phase B was 80% (V / V); From 40 minutes to 40.1 minutes, mobile phase A linearly increased to 90% (V / V), and mobile phase B linearly decreased to 10% (V / V); from 40.1 minutes to 45 minutes,...

Embodiment 2

[0078] Determination of impurities in Apremilast API:

[0079] Prepare about 15mg of this product before using it, weigh it accurately, put it in a 100ml measuring bottle, add 15ml of acetonitrile and shake to dissolve, then use 10mmol / L potassium dihydrogen phosphate solution (take about 1.36g of anhydrous potassium dihydrogen phosphate, add water 1000ml makes dissolving, mixes, and obtains) dilution makes the solution that contains Apremilast about 0.15mg in every 1ml, as need testing solution. Reference substance solution: Take about 7.5 mg of Apremilast reference substance, accurately weighed, put in a 50ml measuring bottle, add 7.5ml of acetonitrile to dissolve, dilute with 10mmol / L potassium dihydrogen phosphate solution to the mark, shake well, and use as For the reference substance stock solution, accurately measure 1ml of the reference substance stock solution, put it in a 100ml measuring bottle, add solvent [acetonitrile-10mmol / L potassium dihydrogen phosphate soluti...

Embodiment 3

[0082] Determination of impurities in apremilast preparations:

[0083] Take an appropriate amount of fine powder of this product (approximately equivalent to 15mg of Apremilast), put it in a 100ml measuring bottle, add 0.01mol / L potassium dihydrogen phosphate solution (take about 1.36g of anhydrous potassium dihydrogen phosphate, add 1000ml of water to dissolve) - 30ml of acetonitrile (volume ratio 50:50), ultrasonic for 5 minutes, add 0.01mol / L potassium dihydrogen phosphate solution to dilute to the mark, shake well, centrifuge, take the supernatant as the test solution. In addition, accurately weigh about 15 mg of Apremilast reference substance, put it in a 100ml measuring bottle, add 15ml of acetonitrile to dissolve, dilute to the mark with 0.01mol / L potassium dihydrogen phosphate solution, shake well, accurately measure 1ml, and put it in 100ml volume In the bottle, add solvent [mixed solution of acetonitrile and 0.01mol / L potassium dihydrogen phosphate solution (volume ...

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Abstract

The invention relates to an apremilast related substance determination method. According to the method, an octadecyl silane bonded silica gel filler chromatographic column is adopted; a buffer solution is used as a mobile phase A, the buffer solution is phosphoric acid, a phosphate solution or a mixture of the phosphoric acid and the phosphate solution, the concentration of the buffer solution is 0.001 mol / L to 0.1 mol / L, and the pH value of the buffer solution is 2.5 to 2.9; acetonitrile is used as a mobile phase B; the flow velocity is 0.8 ml / min to 1.2 ml / min, an ultraviolet detector is used for detection, and gradient elution is carried out. The apremilast related substance determination method is simple in mobile phase system, short in analysis time and high in sensitivity; since the absorption wavelength of known impurities and the detection number of unknown impurities are comprehensively considered, the detectability is better.

Description

technical field [0001] The invention relates to a method for determining related substances, in particular to a method for determining related substances of Apremilast. Background technique [0002] Apremilast (apremilast, (S)-2-[1-(3-ethoxy-4-methoxyphenyl)-2-methanesulfonylethyl]-4-acetylaminoisoindoline -1,3-diketone, molecular formula: C 22 h 24 N 2 o 7 S, molecular weight: 460.5) is an inhibitor of phosphodiesterase-4 (PDE-4). At present, the detection method of related substances is reported in the existing research literature of Apremilast (for example, Chinese patent CN 105588886A). The existing detection methods are insufficient for the research on the synthesis process impurities and degradation products of Apremilast, and the mobile phase system is relatively complex, the analysis time is long, and the sensitivity is low. Contents of the invention [0003] The purpose of the present invention is to address the above-mentioned problems, aiming at a total of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/74
CPCG01N30/02G01N30/34G01N30/74Y02A50/30
Inventor 刘亚元杨明兢冯爱娟朱林任晋生
Owner JIANGSU SIMCERE PHARMA
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