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A kind of calcitriol compound, its preparation method, separation method and application

A separation method, the technology of calcitriol, applied in the direction of organic chemistry, etc., can solve the problems of lack of separation, detection and identification, confirmation of structure, etc.

Active Publication Date: 2021-09-10
SHANGHAI INST OF PHARMA IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the defects in the prior art that lack the separation, detection and identification, and confirmation of the structure of the related substances existing in the calcitriol bulk drug at the same time, and provide a calcitriol compound, Its preparation method, separation method and use

Method used

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  • A kind of calcitriol compound, its preparation method, separation method and application
  • A kind of calcitriol compound, its preparation method, separation method and application
  • A kind of calcitriol compound, its preparation method, separation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0056] (1) Operation in the dark, weigh 1mg of calcitriol raw material, add 300ul of methanol to dissolve, add 200ul of 0.5mol / L NaOH aqueous solution, destroy at 66°C for 1.5h, take it out, cool to room temperature, and dissolve with 1mol / L HCl Methanol solution is neutralized to neutral.

[0057] Operate in a dark place, measure an appropriate amount of the sample after step (1) alkali destruction and neutralization, add methanol to dilute to obtain a sample methanol solution with a concentration of 0.02g / L, measure 20ul of the sample methanol solution obtained, and inject it into a liquid chromatograph. Record the liquid chromatogram and mass spectrometry total ion chromatogram.

[0058] Chromatographic conditions:

[0059] Chromatographic column Capcell Pak C18BB (250mm×4.6mm, 5μm);

[0060] Mobile phase: mobile phase A: 0.02% formic acid aqueous solution, mobile phase B: acetonitrile, linear gradient elution: 0→25min, A:B=45:55; 25→35min, A:B=45:55→10: 90; 35→45min, A:...

Embodiment 2

[0088] 1.1 Solution preparation and detection

[0089] Operation in the dark, preparation and detection of calcitriol sample solution: Accurately weigh an appropriate amount of calcitriol raw material, add methanol to dissolve and dilute to a sample solution with a concentration of 0.1mg / ml. Measure 20 ul of the sample solution, inject it into a liquid chromatograph, adopt the same chromatographic conditions as in Example 1, and record the liquid chromatogram and mass spectrum total ion chromatogram.

[0090] The liquid phase diagram that present embodiment obtains is as Figure 4 As shown, each component is as shown in Table 5, the main peak retention time is suitable, the peak shape is good, and each related substance can be well separated from the main peak. It can be seen from the figure that the method of the present invention can be used to detect calcitriol and its related substances, and the method can be applied to the synthesis process monitoring and quality control...

Embodiment 3

[0094] Because calcitriol is unstable in nature, it is easy to produce isomerization when exposed to light and high temperature, so the reaction conditions need to be controlled to avoid the reduction of the content of target impurities (such as calcitriol compounds shown in formula I) or multiple damages. The influence of temperature, time, solvent and other factors on the degradation reaction was investigated respectively in the following, and the experiment was operated in dark.

[0095] (1) temperature

[0096] To operate in the dark, weigh 1 mg of calcitriol raw material, add 300 ul of methanol to dissolve, add 100 ul of 0.5 mol / L NaOH aqueous solution, destroy it at different temperatures for 1.0 h, take it out, cool to room temperature, and use 1 mol / L HCl methanol The solution is neutralized to neutral.

[0097] Protect from light, take an appropriate amount of the sample after alkali destruction and neutralization, dilute with methanol to obtain a sample methanol sol...

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Abstract

The invention discloses a calcitriol compound, its preparation method, separation method and application. The preparation method comprises the following steps: degrading calcitriol and alkali at 60-80° C. in a solvent, and under the condition of avoiding light. The separation method of the invention can effectively separate the related substances of the calcitriol bulk drug, and has strong method specificity, high sensitivity and strong practicability. The calcitriol compound of the invention is an important reference substance for the quality control of the calcitriol, and can effectively identify the impurities produced in the calcitriol stability test or storage process, thereby controlling the drug quality of the calcitriol.

Description

technical field [0001] The invention relates to a calcitriol compound, its preparation method, separation method and application. Background technique [0002] Calcitriol, also known as active vitamin D3, is the basic form of vitamin D to exert physiological activity in the body. It has the function of regulating calcium and phosphorus in the body. It is suitable for patients with insufficient bone mineralization caused by osteoporosis and renal function damage. [0003] Calcitriol [0004] Due to the unstable nature of calcitriol, isomerization will occur in case of light and high temperature, and its raw material medicine also contains other impurities. Therefore, it is necessary to analyze its related substances. At present, there are few studies on calcitriol-related substances at home and abroad, and it is urgent to study them to improve the quality of calcitriol products. Contents of the invention [0005] The technical problem to be solved by the present invent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C401/00
CPCC07C401/00C07C2601/16C07C2602/24
Inventor 李悦陆静陈泽蔡鹏俊
Owner SHANGHAI INST OF PHARMA IND CO LTD
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