A kind of high performance liquid chromatography analysis method of pomalidomide related substance

A technology of high-performance liquid chromatography and analysis method, which is applied in the field of analysis of the purity of chemical drugs, can solve the problems of no relevant literature reports, etc., and achieve the effect of great positive progress, great practical application value, and strong method specificity

Active Publication Date: 2019-01-04
HEFEI JIUNUO MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, there is no relevant literature report on the analysis method of pomalidomide raw material and its preparation based on comprehensive impurity profile analysis

Method used

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  • A kind of high performance liquid chromatography analysis method of pomalidomide related substance
  • A kind of high performance liquid chromatography analysis method of pomalidomide related substance
  • A kind of high performance liquid chromatography analysis method of pomalidomide related substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Detection equipment and chromatographic conditions:

[0042] High performance liquid chromatography: LC-10AD pump, SPD-M10A detector

[0043] Chromatographic column: Agilent C18 (150×4.6mm, 5μm); mobile phase A: acetonitrile-water-phosphoric acid solution with a volume ratio of 5:95:0.1; mobile phase B: acetonitrile-water with a volume ratio of 25:75:0.1 - Phosphoric acid solution; detection wavelength: 226nm; flow rate: 1.0ml / min; injection volume: 20μl.

[0044] Experimental steps:

[0045] (1) Sample preparation:

[0046] Take an appropriate amount of pomalidomide and known impurities A-I, add an acetonitrile-water-phosphoric acid solution with a volume ratio of 50:50:0.1 to ultrasonically dissolve and quantitatively dilute the mixed solution to an appropriate concentration, shake well, and use it as a sample solution.

[0047] (2) Gradient elution program setting:

[0048] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

100

0

...

Embodiment 2

[0052] Detection equipment and chromatographic conditions:

[0053] High performance liquid chromatography: LC-10AD pump, SPD-M10A detector

[0054] Chromatographic column: Agilent C18 (150×4.6 mm, 5 μm); mobile phase A: same as Example 1, mobile phase B: same as Example 1; flow rate: 1.0 ml / min; detection wavelength: 226 nm; injection volume: 20 μl.

[0055] (1) Sample preparation:

[0056] Acid destruction: Take the contents of pomalidomide capsules, grind them finely, take an appropriate amount of fine powder (about 20 mg containing pomalidomide), put it in a 100ml measuring bottle, add 4ml of 1mol / L hydrochloric acid solution, and put it in a water bath at 100°C for 1 hour. After 1 hour, take it out and let it cool, add 4ml of 1mol / L sodium hydroxide solution to neutralize it, add an appropriate amount of acetonitrile-water-phosphoric acid solution with a volume ratio of 50:50:0.1 to sonicate to dissolve and dilute to the mark, shake well, filter, and use as acid damage ...

Embodiment 3

[0066] Detection equipment and chromatographic conditions:

[0067] High performance liquid chromatography: UltiMate 3000 pump, UltiMate 3000 UV detector

[0068] Chromatographic column: Agilent C18 (150×4.6 mm, 5 μm); mobile phase A: same as Example 1, mobile phase B: same as Example 1; flow rate: 1.0 ml / min; detection wavelength: 226 nm; injection volume: 20 μl.

[0069] Experimental steps:

[0070] (1) Sample preparation: Take 20 mg of pomalidomide, put it in a 100 ml measuring bottle, dissolve it ultrasonically with an acetonitrile-water-phosphoric acid solution with a volume ratio of 50:50:0.1, dilute to the mark, shake well, and use it as a sample solution.

[0071] (2) Gradient elution program setting:

[0072] time (minutes)

Mobile phase A(%)

Mobile phase B(%)

0

100

0

2

100

0

15

0

100

40

0

100

41

100

0

50

100

0

[0073] (3) Detection: Take the above-mentioned sample solutio...

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Abstract

The invention discloses a high performance liquid chromatography method of pomalidomide related substance. The method includes: using a reverse phase chromatographic column and an ultraviolet detector; using acetonitrile-water-phosphoric acid as a mobile phase for gradient elution.by using the method, all known impurities in pomalidomide raw materials and preparations thereof can be analyzed at the same time, content of each known impurity can be effectively controlled through a comparison method of main ingredients added with a correction factor, separation degrees among impurity peaks and between main peaks and adjacent impurity peaks are all greater than 1.5, and peak purity of the main peaks and the impurity peaks is 1.0. A simple and reliable analysis method is provided for quality control analysis of the pomalidomide raw materials and the preparations thereof.

Description

1. Technical field [0001] The invention relates to a method for analyzing the purity of chemical drugs, in particular to a method for analyzing pomalidomide related substances by high performance liquid chromatography. 2. Background technology [0002] Pomalidomide (Macitentan), chemical name (RS)-4-amino-2-(2,6-dioxopiperidin-3-yl)-isoindoline-1,3-dione, chemical structural formula as follows: [0003] [0004] Pomalidomide is the third immunomodulator drug after thalidomide and lenalidomide developed by Celgene in the United States. It is suitable for patients who have received at least two drug treatments in the past [including Multiple myeloma patients with lenalidomide and bortezomib] and disease progression on or within 60 days of treatment completion. [0005] The general synthesis method of pomalidomide has been disclosed in patents US2007004920 and US5635517. According to the analysis of the synthesis process, its impurities mainly come from the reaction raw ma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 吴标李晓梅施伶俐崔红晓
Owner HEFEI JIUNUO MEDICAL TECH
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