Method for detecting content of 3, 3, 20, 20-bis(ethylenedioxy)-17alpha-hydroxy-19-norpregna-5(10),9(11)-diene in ulipristal acetate intermediate I

A technology of ulipristal acetate and intermediates, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as difficulties, and achieve the effect of simple operation, good selectivity, and better separation effect

Inactive Publication Date: 2021-03-30
HUNAN NORCHEM PHARMACEUTICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the similar structures of Ubiketal and Ulipristal Acetat...

Method used

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  • Method for detecting content of 3, 3, 20, 20-bis(ethylenedioxy)-17alpha-hydroxy-19-norpregna-5(10),9(11)-diene in ulipristal acetate intermediate I
  • Method for detecting content of 3, 3, 20, 20-bis(ethylenedioxy)-17alpha-hydroxy-19-norpregna-5(10),9(11)-diene in ulipristal acetate intermediate I
  • Method for detecting content of 3, 3, 20, 20-bis(ethylenedioxy)-17alpha-hydroxy-19-norpregna-5(10),9(11)-diene in ulipristal acetate intermediate I

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Embodiment 1

[0025] A method for detecting ulinastal ketal content in ulipristal acetate intermediate I, comprising the steps,

[0026] 1. The chromatographic column is Welch Ultimate XB-C18 250*4.6mm, 5μm particle size or similar chromatographic column.

[0027] 2. The detection wavelength is 235nm, which is the wavelength at which ulipristal acetate intermediate Ⅰ and ulinacetal have relatively large absorption in the ultraviolet-visible region.

[0028] 3. Through the optimized gradient elution procedure, as follows:

[0029]

[0030] 4. The analysis time is 2.0 times the retention time of the main peak.

[0031] 5. Use the area normalization method to calculate the content of ulipristal acetate intermediate I; the injection volume is 10ul; the flow rate is 1.0ml / min; the column temperature is 35°C.

[0032] 6. Orthodione positioning solution: Accurately weigh an appropriate amount of ureadione, accurately weigh it, dissolve and dilute it with acetonitrile to make a solution contai...

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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 3, 3, 20, 20-bis(ethylenedioxy)-17alpha-hydroxy-19-norpregna-5(10),9(11)-diene in an ulipristal acetate intermediate I. The method comprises the following steps: preparing a test solution; preparing a reference substance solution of 3, 3, 20, 20-bis(ethylenedioxy)-17alpha-hydroxy-19-norpregna-5(10),9(11)-diene; wherein chromatographic conditions are shown as follows: octadecylsilane is used as a stationary phase, a mobile phase is selected for gradient elution, and the detection wavelength is 235 nm; wherein the mobile phase A is a tetrabutylammonium hydrogen sulfate solution with the mass concentration of 0.01%-0.1% or a lauryl sodium sulfate solution with the mass concentration of 0.01%-0.1%, and the mobile phase B is acetonitrile; determining the content. The detection result is accurate, and the detection method is efficient, quick and sensitive, so that the quality of the ulipristal acetate finished product is improved.

Description

technical field [0001] The invention belongs to the field of organic substance content detection, and in particular relates to a method for detecting the content of ulinadiketal in ulipristal acetate intermediate I. Background technique [0002] Ulipristal acetate [3,3,20,20-bis(ethylenedioxy)-17α-hydroxy-19-norpregna-5(10),9(11 )-diene] synthesis of ulipristal acetate intermediate Ⅰ (3,3,20,20-bis(ethylenedioxy)-17A-hydroxyl-5A (epoxide)) was synthesized as ulipristal acetate The key reaction step, and the residual amount of ulinastal ketal directly affects the quality of ulipristal acetate finished product, so the content of ulinastal ketal must be controlled in ulipristal acetate intermediate Ⅰ. Since the structure of uridine ketal is similar to the structure of ulipristal acetate intermediate I, it is difficult to separate the two by general separation methods, so a specific and sensitive method is required to ensure the determination The results are accurate and relia...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/60G01N30/74
CPCG01N30/02G01N30/06G01N30/34G01N30/60G01N30/36G01N30/74
Inventor 李林梅曾春玲靳志忠张跃杨姣
Owner HUNAN NORCHEM PHARMACEUTICAL CO LTD
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