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Method of separation and detection of apremilast and enantiomer thereof by adopting HPLC (high performance liquid chromatography)

A high-performance liquid chromatography and enantiomer technology, applied in the field of analytical chemistry, can solve the problems of low resolution, inability to separate enantiomers, poor separation effect, etc., and achieve high sensitivity and high column efficiency Effect

Inactive Publication Date: 2015-12-09
宜邦国创药物研究院(北京)有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Enantiomers cannot be separated by conventional high performance liquid chromatography and must be separated using a suitable chiral column
[0005] Chinese patent 201410765717.5 discloses a method for related substances of Apremilast, which uses an AD-H chromatographic column, and the mobile phase is n-hexane / isopropanol / diethylamine / trifluoroacetic acid=80 / 20 / 0.2 / 0.5 , flow rate 1.0mL / min, column temperature 40°C, detection wavelength 240nm, but the resolution of this method is low
However, the separation effect of this method is not good when using ChiralPakAD-H chromatographic column, and the separation effect is better when using AS-H chromatographic column, but this type of chromatographic column is expensive

Method used

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  • Method of separation and detection of apremilast and enantiomer thereof by adopting HPLC (high performance liquid chromatography)
  • Method of separation and detection of apremilast and enantiomer thereof by adopting HPLC (high performance liquid chromatography)
  • Method of separation and detection of apremilast and enantiomer thereof by adopting HPLC (high performance liquid chromatography)

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Embodiment 1

[0021] Instruments and Conditions

[0022] High performance liquid chromatography: Agilent1260

[0023] Chromatographic column: ChiralPakAD-H (250*4.6mm, 5μm)

[0024] Mobile phase: hexane-ethanol-acetonitrile-diethylamine (45:45:10:0.1)

[0025] Flow rate: 0.8ml / min

[0026] Wavelength: 230nm

[0027] Column temperature: 35°C

[0028] Injection volume: 10μL

[0029] Experimental steps:

[0030] Take 5 mg of Apremilast, add 1 ml of acetonitrile to dissolve, dilute with ethanol to make a solution containing about 1.0 mg per 1 ml, as the test solution; take 5 mg of Apremilast racemate, add 1 ml of acetonitrile to dissolve, use Dilute with ethanol and make a solution containing about 1.0mg per 1ml, take 10μl into the liquid chromatograph, record the chromatogram, accurately measure 10μl of the test solution, inject it into the liquid chromatograph, and record the chromatogram.

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Abstract

The invention discloses a method of separation and detection of apremilast and enantiomer thereof by adopting HPLC (high performance liquid chromatography). The chromatographic condition of the method adopts a chiral column taking a silica gel of which the surface is coated with amylose-three(3,5-dimethyl phenyl carbamate) as filler; a mobile phase is prepared from hexane-ethyl alcohol-acetonitrile-diethylamine (the ratio is 45 to 45 to 10 to 0.1); the flow velocity is 0.8ml / min; the wavelength is 230nm; and the column temperature is 35 DEG C.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring apremilast and its enantiomers by high-performance liquid chromatography. Background technique [0002] Apremilast is a phosphodiesterase inhibitor. It is the first small-molecule drug approved by the FDA on March 21, 2014 for the treatment of arthritis caused by psoriasis. The original research company is Celgene. The chemical structural formula is as follows: [0003] [0004] Separation of enantiomers containing chiral carbon atoms has always been a difficult point in quality control during the synthesis and preparation of chiral drugs. Apremilast is a chiral drug. In order to ensure the safety of the drug, it is necessary to detect the content of enantiomer impurities in the drug in the quality standard. Enantiomers cannot be separated by conventional high-performance liquid chromatography and must be separated using a...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 张在富吴浩山许馨文
Owner 宜邦国创药物研究院(北京)有限公司
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