Chromatographic separation method of progesterone intermediate II and progesterone intermediate I and quantitative detection method of progesterone intermediate II and progesterone intermediate I

A technique for chromatographic separation and intermediates, which is applied in the field of material separation, can solve the problems of unpublished reports of separation and quantitative detection methods, separation, and no separation methods, and achieves fast and simple determination, easy operation, and improved selectivity. Effect

Inactive Publication Date: 2019-05-28
湖南成大生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the similar structure of intermediate Ⅰ and intermediate Ⅱ, it is difficult to separate the two by general separation methods. At present, there is no simple and easy separation method, and there are no public reports of progesterone intermediate Ⅱ and intermediate Ⅱ at home and abroad. Separation of progesterone intermediate Ⅰ and quantitative detection method of progesterone intermediate Ⅰ

Method used

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  • Chromatographic separation method of progesterone intermediate II and progesterone intermediate I and quantitative detection method of progesterone intermediate II and progesterone intermediate I
  • Chromatographic separation method of progesterone intermediate II and progesterone intermediate I and quantitative detection method of progesterone intermediate II and progesterone intermediate I
  • Chromatographic separation method of progesterone intermediate II and progesterone intermediate I and quantitative detection method of progesterone intermediate II and progesterone intermediate I

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Experimental program
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Effect test

Embodiment 1

[0060] 1) Chromatographic conditions: the chromatographic column is Agela promosil C18, 250mm*4.6mm, and the stationary phase is octadecylsilane with a particle size of 5 μm.

[0061] 2) The detection wavelength is 240nm, which is the wavelength at which both progesterone intermediate II and intermediate I have large absorption in the ultraviolet and visible light region.

[0062] 3) The mobile phase and gradient elution program are as follows in Table 1:

[0063] Table 1

[0064] time / min

Acetonitrile V% in mobile phase

0.1wt% phosphoric acid V% in mobile phase

0-30

60

40

30-35

60→85

40→15

35-45

85

15

45-50

85→60

15→40

50-55

60

40

[0065] 4) The total analysis time is 55 minutes.

[0066] 5) Obtain the correction factor; Dissolve and dilute the progesterone intermediate II with acetonitrile to make the following concentration, and then carry out chromatographic analysis under the following ch...

Embodiment 2

[0075] Example 2 is basically the same as Example 1, except that 0.1 wt% phosphoric acid in the mobile phase is replaced by 0.1 wt% trifluoroacetic acid. The obtained chromatographic absorption spectrum is as Figure 4 As shown, other parameters of its peak structure are shown in Table 4. Among them, when the retention time of progesterone intermediate II is about 2 min, it has multiple peaks; the position of the retention time of progesterone intermediate I is about 36.052 min.

[0076] Table 4

[0077]

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Abstract

The invention relates to a chromatographic separation method of progesterone intermediate II and progesterone intermediate I and a quantitative detection method of progesterone intermediate II and progesterone intermediate I. Octadecylsilane is used as a stationary phase, and acetonitrile-0.1 wt%- 0.5 wt% of an acid solution is used as a mobile phase. The elution gradient of mobile phase is as follows: in 0-30 min, the volume content of the acetonitrile is 60%, and the volume content of the acid solution is 40%; the volume content of the acetonitrile is increased from 60% to 85% and the volumecontent of the acid solution is decreased from 40% to 15% in 30-35min; in 35-45min, the volume content of the acetonitrile is 85%, and the volume content of the acid solution is 15%; in 45-50min, thevolume content of the acetonitrile is decreased from 85% to 60%, and the volume content of the acid solution is increased from 15% to 40%; in 50-55 min, the volume content of the acetonitrile is 60%,and the volume content of the acid solution is 40%. The chromatographic separation method of the progesterone intermediate II and the progesterone intermediate I and the quantitative detection methodof the progesterone intermediate II and the progesterone intermediate I are easy to operate, and the separation efficiency is improved, and the accuracy of content determination is improved.

Description

technical field [0001] The invention relates to the technical field of substance separation, in particular to a chromatographic separation method and a quantitative detection method of progesterone intermediate II and progesterone intermediate I. Background technique [0002] In the production process of progesterone, intermediate Ⅰ (20-formyl progesterone-4-en-3-one) synthesizes intermediate Ⅱ (20-methine-((E)-1-piperidine) progesterone- 4-en-3-one) is a key reaction step in the synthesis of progesterone, and the residual amount of intermediate I directly affects the quality of the finished product of progesterone, so the intermediate I must be controlled when the crude product of progesterone intermediate II is obtained. content. However, due to the similar structure of intermediate Ⅰ and intermediate Ⅱ, it is difficult to separate the two by general separation methods. At present, there is no simple and easy separation method, and there are no public reports of progester...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): B01D15/08B01D15/42G01N30/02G01N30/34G01N30/60G01N30/74
Inventor张跃童志杰刘喜荣
Owner湖南成大生物科技有限公司