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Method for detecting content of impurities in ulipristal acetate intermediate II

A technology for ulipristal acetate and impurity content, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve good selectivity, fast and simple determination, and good separation

Active Publication Date: 2021-03-09
HUNAN NORCHEM PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no public report at home and abroad on the analytical method for the determination of ulipristal acetate intermediate Ⅰ in ulipristal acetate intermediate Ⅱ

Method used

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  • Method for detecting content of impurities in ulipristal acetate intermediate II
  • Method for detecting content of impurities in ulipristal acetate intermediate II
  • Method for detecting content of impurities in ulipristal acetate intermediate II

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Embodiment 1

[0031] A method for detecting impurity content in ulipristal acetate intermediate II, comprising the steps of,

[0032] 1. The chromatographic column is Agela promosil C18 250*4.6mm, 5μm particle size or similar chromatographic column.

[0033] 2. The detection wavelength is 240nm. Ulipristal acetate intermediate II and impurities C-D all have relatively large absorption wavelengths in the ultraviolet-visible region.

[0034] 3. Through the optimized gradient elution procedure, as follows:

[0035]

[0036] 4. The analysis time is 75 minutes.

[0037] 5. The content of ulipristal acetate intermediate II was normalized by the area normalization method; the injection volume was 10ul; the flow rate was 1.0ml / min; the column temperature was 35°C.

[0038] 6. Impurity C / D positioning solution: Accurately weigh the appropriate amount of Ulipristal Acetate Impurities C to D, accurately weigh, dissolve and dilute with acetonitrile to make a solution containing about 1mg per 1ml, ...

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Abstract

The invention belongs to the field of organic substance content detection, and particularly relates to a method for detecting the content of ulipristal diketal in an ulipristal acetate intermediate I.The method comprises the following steps that: a test solution is prepared; an impurity reference substance solution is prepared; under chromatographic conditions, octadecylsilane is taken as a stationary phase, a mobile phase is selected for isocratic elution, and the detection wavelength is 220-240nm; a mobile phase A is a phosphoric acid solution with the mass concentration of 0.01%-0.05%, a glacial acetic acid solution with the mass concentration of 0.01%-0.05%, a trifluoroacetic acid solution with the mass concentration of 0.01%-0.05% or a formic acid solution with the mass concentrationof 0.01%-0.05%, and a mobile phase B is acetonitrile; and an elution procedure is limited, the content is determined, the test solution and the impurity reference substance solution are sucked and injected into a high performance liquid chromatograph, and the content of impurities C and D is determined. The content of the impurities can be accurately, quickly and efficiently determined, and the sensitivity is high.

Description

technical field [0001] The invention belongs to the field of detection of organic substance content, and in particular relates to a method for detection of impurity content in ulipristal acetate intermediate II. Background technique [0002] In the production process of ulipristal acetate, intermediate Ⅰ[3,3,20,20-bis(ethylenedioxy)-17Α-hydroxy-5Α(epoxide)] synthesizes intermediate Ⅱ[(11B)- 11-[4-(Dimethylamino)phenyl]-5,17-dihydroxy-19-desmethylandrost-9-ene-3,20-dione bis(1,2-ethylene glycol) Cyclic acetal (Grignard product)] is a key reaction step in the synthesis of ulipristal acetate. During the reaction process, there are impurities in the following table 1, which are respectively impurity C (process by-product) and impurity D (process by-product). [0003] Table 1 Possible impurities in ulipristal acetate intermediate Ⅱ [0004] [0005] The residual amount of these two impurities directly affects the quality of ulipristal acetate finished product, so the conten...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/60G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/8679G01N30/60
Inventor 李林梅张跃曾春玲靳志忠杨姣
Owner HUNAN NORCHEM PHARMACEUTICAL CO LTD
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