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A method for detecting impurity content 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, easy operation, and good separation

Active Publication Date: 2022-02-22
HUNAN NORCHEM PHARMACEUTICAL CO LTD
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  • 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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  • A method for detecting impurity content in ulipristal acetate intermediate II
  • A method for detecting impurity content in ulipristal acetate intermediate II
  • A method for detecting impurity content 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 detection of organic substance content, and in particular relates to a method for detecting the content of ulinadiketal in ulipristal acetate intermediate I, comprising the following steps: preparing a test solution; preparing an impurity reference solution; chromatographic conditions, Using octadecylsilyl as the stationary phase, the mobile phase is selected for isocratic elution, and the detection wavelength is 220-240nm; the mobile phase A is 0.01%-0.05% mass concentration phosphoric acid solution, 0.01%-0.05% mass concentration glacial acetic acid Solution, 0.01%-0.05% mass concentration trifluoroacetic acid solution or 0.01%-0.05% mass concentration formic acid solution, the mobile phase B is acetonitrile; limit the elution procedure, measure the content, draw the test solution and the impurity reference solution, inject The high-performance liquid chromatograph measures the content of impurities C and D. The invention can accurately, quickly and efficiently measure the content of impurities with high sensitivity.

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 Patents(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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