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Method for separating and measuring Apremilast and enantiomer of Apremilast through liquid chromatography

A liquid chromatography and enantiomer technology, applied in the field of separation and determination of apremilast and its corresponding isomers by liquid chromatography, can solve the problems of small separation, low sensitivity, low column efficiency, etc. Accurate separation and detection, simple determination method, and the effect of quality control

Active Publication Date: 2016-06-01
安徽瑞达健康产业有限公司
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Problems solved by technology

[0004] It is difficult to effectively separate apremilast and its enantiomers by the determination method of high performance liquid chromatography using conventional general chiral columns and conventional mobile phases, the column efficiency is very low, and the peak shape is very poor
Enantiomers cannot be separated by conventional high performance liquid chromatography and must be separated using appropriate methods
[0005] Chinese patent 20150253092.9 discloses a method for the separation and detection of Apremilast and its enantiomers. The method uses a ChiralPakAD-H chromatographic column, and the mobile phase is n-hexane-dehydrated alcohol-diethylamine=50:50: 0.1, flow rate 1.0ml / min, column temperature 25°C, detection wavelength 240nm, but this method has low sensitivity and low resolution

Method used

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  • Method for separating and measuring Apremilast and enantiomer of Apremilast through liquid chromatography
  • Method for separating and measuring Apremilast and enantiomer of Apremilast through liquid chromatography
  • Method for separating and measuring Apremilast and enantiomer of Apremilast through liquid chromatography

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Embodiment

[0036] 1. Instruments and conditions

[0037] Instrument: Shimadzu LC-15C High Performance Liquid Chromatograph

[0038] Chromatographic column: ChiralPakID (5um, 250×4.6mm)

[0039] Mobile phase: methyl tert-butyl ether-ethanol-diethylamine=91:9:0.1

[0040] Detection wavelength: 230nm

[0041] Flow rate: 1.0ml / min

[0042] Column temperature: 30°C

[0043] Injection volume: 10ul

[0044] The sample injection of the present invention is manual sample injection.

[0045] 2. Experimental steps

[0046] Take 5 mg of Apremilast reference substance, accurately weigh it, place it in a 10ml volumetric flask, add an appropriate amount of absolute ethanol, and heat it in a water bath at a temperature of 45°C for an appropriate amount of time to dissolve it; dilute and set the volume to The solution containing 0.5mg in every 1ml is used as the reference substance solution; take 10mg of Apremilast, accurately weigh it, place it in a 10ml volumetric flask, add an appropriate amoun...

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Abstract

The invention provides a method for separating and measuring Apremilast and enantiomer of the Apremilast through liquid chromatography, and relates to the technical field of analytical chemistry. The method comprises the steps that a chiral chromatographic column with silica gel as filler is adopted, the surface of the silica gel is in covalent bonding with amylase-tris(3-chlorobenzene carbamate), methyl tertiary butyl ether-ethyl alcohol-diethylamine (91-9-0.1) serves as a mobile phase, the flow speed is 1 ml / min, the wave length is 230 nm, and the column temperature is 30 DEG C. The high performance liquid chromatography separating and detecting method for the Apremilast and the enantiomer of the Apremilast is high in separation degree and high in specificity, the problem that the Apremilast and corresponding isomer of the Apremilast are hard to separate is solved, and therefore it is guaranteed that the quality of the Apremilast and a preparation of the Apremilast is controllable.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a method for separating and measuring apremilast and its corresponding isomers by liquid chromatography. Background technique [0002] Apremilast is an inhibitor of phosphodiesterase-4 (PDE-4), which is developed by the American company Celgene and is mainly used for the treatment of psoriasis-induced arthritis. Its chemical name is: N-{2-[(1S)-1-(3-ethoxy-4-methoxyphenyl)-2-(methylsulfonyl)ethyl]-2,3-dihydro-1,3 -Dioxo-1H-isoindol-4-yl}acetamide, its molecular formula is C22H24N2O7S, and its chemical structure is as follows: [0003] [0004] It is difficult to effectively separate apremilast and its enantiomers by the high-performance liquid chromatography method using conventional general chiral columns and conventional mobile phases, the column efficiency is very low, and the peak shape is very poor. Enantiomers cannot be separated by conventional high perfo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 王娜娜
Owner 安徽瑞达健康产业有限公司
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