Method for detecting enantiomer impurity in apremilast

A technology for enantiomers and detection methods, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of reduced column efficiency, chromatographic column damage, and short service life, and achieves excellent linearity and long service life. Long, easy-to-operate effect

Inactive Publication Date: 2016-04-13
CHENGDU BAIYU JINGELAI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because starch is water soluble, the mobile phase must be absolutely anhydrous to ensure column lifetime
Inevitably, after a long period of use, this type of chromatographic column will be damaged and its service life will be short
[0008] I

Method used

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  • Method for detecting enantiomer impurity in apremilast
  • Method for detecting enantiomer impurity in apremilast
  • Method for detecting enantiomer impurity in apremilast

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] 1. Determination of detection wavelength

[0053] Take Apremilast tablets, grind finely, accurately weigh an appropriate amount, and use mobile phase (methyl tert-butyl ether-n-butanol=75:25) to prepare a solution with a concentration of 20 μg / mL as the test solution.

[0054] Accurately weigh an appropriate amount of the reference substance (enantiomer), and use a mobile phase (methyl tert-butyl ether-n-butanol=75:25) to prepare a solution with a concentration of 20 μg / mL as the reference substance solution.

[0055] Take the above-mentioned test solution and reference solution, and scan in the wavelength range of 200nm to 400nm. The test results are shown in Table 1.

[0056] Table 1, the ultraviolet scanning result of the present invention

[0057] project

Peak wavelength(nm)

peak

Valley wavelength(nm)

valley

Test solution

230

0.617

215

0.226

Reference solution

230

0.775

296

0.010

[0058]...

Embodiment 2

[0118] Detection by normal phase high performance liquid chromatography:

[0119] Chromatographic column: a chromatographic column filled with α-acid glycoprotein-bonded silica gel;

[0120] The model of the chromatographic column is CHIRALAGP, and the specifications are: the inner diameter is 4.6mm, the length is 150mm, and the filler particle size is 5μm;

[0121] Mobile phase: methyl tert-butyl ether-n-butanol (75:25);

[0122] Column temperature: 35°C;

[0123] Flow rate: 1.0mL / min;

[0124] Detection wavelength: 230nm;

[0125] Injection volume: 20 μL.

[0126] Carry out system suitability test according to the method for embodiment 1, the result shows: apremilast (retention time is 6.353min) and enantiomer (for its retention time is 5.345min) the degree of separation is 3.654, theoretical The number of plates (calculated by Aprester peak) is 7349, and the tailing factor of Aprester peak is 0.975.

[0127] It can be seen that the chromatographic conditions can accur...

Embodiment 3

[0129] Detection by normal phase high performance liquid chromatography:

[0130] Chromatographic column: a chromatographic column filled with α-acid glycoprotein-bonded silica gel;

[0131] The model of the chromatographic column is CHIRALAGP, and the specifications are: the inner diameter is 4.6mm, the length is 150mm, and the filler particle size is 5μm;

[0132] Mobile phase: methyl tert-butyl ether-n-butanol (70:30);

[0133] Column temperature: 35°C;

[0134] Flow rate: 1.0mL / min;

[0135] Detection wavelength: 230nm;

[0136] Injection volume: 20 μL.

[0137] Carry out system suitability test according to the method for embodiment 1, the result shows: the separation degree between apremilast (retention time is 10.115min) and enantiomer (for its retention time is 8.725min) is 4.128, theoretical The plate number (according to Aprester peak calculation) is 8107, and the tailing factor of Aprester peak is 1.08.

[0138] It can be seen that the chromatographic conditio...

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Abstract

The invention discloses a method for detecting an enantiomer (I) in apremilast. A protein type chiral chromatographic column is adopted in the method; while the defect of shorter service life of an existing starch coating chiral column is overcome, the enantiomer in the apremilast is effectively separated and detected, and a detection result is accurate and reliable; the method has the multiple advantages such as excellent linear relation, high precision, good stability, good repeatability, good recovery rate, simple and convenient operation and low cost, and is suitable for popularization and application. A structural formula is shown in the description.

Description

technical field [0001] The invention relates to a method for detecting enantiomer impurities in 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) was developed by Celgene Biotechnology Company of the United States, and was approved by the U.S. Food and Drug Administration (FDA) for the treatment of active psoriatic arthritis (PsA) in adults on March 21, 2014. named Otezla. [0003] [0004] Apremilast is a chiral drug, and its effective configuration is the S configuration. Therefore, in Apremilast products, the existence of its R configuration isomer impurity (I) will seriously affect the drug safety and clinical effect of the product, and it is necessary to detect the content of impurity (I) in Apremilast , to effectively monitor the quality of Apremilast. [0005] Chinese patent CN10...

Claims

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Application Information

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IPC IPC(8): G01N30/74G01N30/60G01N30/06
CPCG01N30/74G01N30/06G01N30/60
Inventor 宋务雄孙毅
Owner CHENGDU BAIYU JINGELAI PHARMA CO LTD
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