Method for separating and determining calcipotriol intermediate F and impurities thereof

A technology of calcipotriol and intermediates, applied in the field of analytical chemistry, to achieve the effect of ensuring product quality, strong specificity, and high sensitivity

Active Publication Date: 2016-06-29
CHONGQING HUAPONT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] There is no published method to report the method for separation and determination of calcipotriol intermediate F and its impurities

Method used

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  • Method for separating and determining calcipotriol intermediate F and impurities thereof
  • Method for separating and determining calcipotriol intermediate F and impurities thereof
  • Method for separating and determining calcipotriol intermediate F and impurities thereof

Examples

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Embodiment 1

[0055] (1) Instruments and conditions

[0056] Instrument: high performance liquid chromatography

[0057] Chromatographic column: ODSHYPERSIL (250×4.0mm, 5um)

[0058] Mobile phase: mixed solution of methanol and ethyl acetate

[0059] The volume ratio of methanol to ethyl acetate is 9:1

[0060] Wavelength: 270nm

[0061] Column temperature: 25°C

[0062] Flow rate: 1.5ml / min

[0063] Injection volume: 20μl

[0064] Diluent: Mixed solution of methanol and ethyl acetate

[0065] The volume ratio of methanol to ethyl acetate is 8:2

[0066] (2) Experimental steps

[0067] a) Impurity VD2 reference solution: Take 9.88mg of VD2 reference substance, put it in a 50ml measuring bottle, add 10ml of ethyl acetate to dissolve, add methanol to dilute to the mark, shake well, and you get it.

[0068] b) Impurity E control solution: take 10.14 mg of impurity E reference substance, put it in a 50 ml measuring bottle, add 10 ml of ethyl acetate to dissolve, add methanol to dilute ...

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Abstract

The invention belongs to the field of analytical chemistry, and particularly relates to a method for separating and determining a calcipotriol intermediate F and impurities thereof. According to the method, solid-liquid separation is performed by adopting octadecylsilane chemically bonded silica as a chromatographic column of a filling agent and taking a mixed solution of methanol and ethyl acetate as a mobile phase, and the impurities comprise one or more of VD2, E, D and an isomer F' of F; effective separation of the intermediate F and the enantiomer impurity thereof can be achieved, effective separation of the intermediate F and the other impurities also can be achieved, the content of the intermediate F and the impurities thereof can be further accurately determined, and the specificity and the sensitivity are high. The operation method is simple, has the advantages of being simple, convenient and rapid and has the extremely important significance on quality control and safety guarantee of the calcipotriol intermediate F.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for separating and measuring calcipotriol intermediate F and impurities thereof. Background technique [0002] Calcipotriol is a derivative of vitamin D, which can inhibit the excessive proliferation of skin cells (keratinocytes) and induce their differentiation, so that the abnormal proliferation and differentiation of psoriatic skin cells can be corrected. local treatment. [0003] Calcipotriol intermediate F is an important intermediate for the synthesis of calcipotriol, and its structural formula is as follows: [0004] [0005] In order to control the quality of the calcipotriol intermediate F, it is necessary to separate and measure the calcipotriol intermediate F and its impurities. When synthetic calcipotriol intermediate F, can produce the isomer F ' of impurity VD2, E, D and F, their structural formula is as follows: [0006] [0007] Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02C07F7/18C07C401/00
CPCC07C401/00C07F7/1804G01N30/02G01N2030/027
Inventor 杨婧周春燕曾正英
Owner CHONGQING HUAPONT PHARMA
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