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Calcium cantharidinate and preparation method thereof

A technology of calcium cantharidinate and cantharidin, which is applied in the field of chemistry, can solve the problem of reduced anticancer activity, and achieve the effects of small molecular weight, strong antitumor effect, and high purity

Inactive Publication Date: 2013-04-17
ZUNYI MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when sodium cantharidinate reduces toxicity, its anticancer activity decreases greatly, which urgently requires the development of other new cantharidin derivatives with higher anticancer activity to solve this problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] A preparation method of calcium cantharidinate, comprising the steps of:

[0015] (1) Add 1g of pure cantharidin into a 50ml Erlenmeyer flask, add 30ml of chloroform solution, heat to dissolve, and at the same time take 0.2g of calcium hydroxide and add 30ml of distilled water to make a suspension;

[0016] (2) Add the calcium hydroxide suspension to the chloroform solution in which cantharidin is dissolved, heat to 60°C, evaporate the chloroform to dryness, and filter to obtain a white suspension; put it in an oven to concentrate and dry to obtain a white crystalline powder;

[0017] (3) Add 30ml of chloroform to the white crystalline powder, heat to 40°C for 2 hours to dissolve the cantharidin, filter, and dry to obtain the white crystalline powder, which is pure calcium cantharidinate.

Embodiment 2

[0019] A preparation method of calcium cantharidinate, comprising the steps of:

[0020] (1) Add 1g of pure cantharidin into a 100ml Erlenmeyer flask, add 50ml of isopropanol solution, heat to dissolve, and at the same time take 0.2g of calcium hydroxide and add 30ml of distilled water to make a suspension;

[0021] (2) Add the calcium hydroxide suspension to the isopropanol solution in which cantharidin is dissolved, heat to 75°C, evaporate the isopropanol to dryness, and filter to obtain a white suspension; put it in an oven to concentrate and dry to obtain a white crystalline powder;

[0022] (3) Add 50ml of isopropanol to the white crystalline powder (or add the white crystalline powder to 50ml of isopropanol), heat to 40°C for 2 hours to dissolve cantharidin, filter, and dry to obtain white The crystalline powder is pure calcium cantharidinate.

experiment example 1

[0023] Experimental Example 1: Product Purity Check

[0024] There is no national quality determination standard for calcium cantharidinate, so it is measured with reference to the national drug standard for sodium cantharidinate [standard number: WS-10001-(HD-0044)-2002].

[0025] Assay

[0026] Chromatographic conditions and system suitability test Octadecylsilane bonded silica gel was used as filler; methanol-water (51:49) was used as mobile phase; flow rate was 1.0ml / min; detection wavelength was 227nm; sensitivity was 0.005AUFS. The number of theoretical plates is calculated based on the peak of cantharidin and should not be less than 2000.

[0027] Preparation of reference substance solution: Take an appropriate amount of cantharidin reference substance, accurately weighed, add methanol to make a solution containing 0.15 mg of cantharidin per 1 ml, as the reference substance solution.

[0028] Preparation of the test solution: Accurately weigh 10mg of this produ...

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PUM

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Abstract

The invention discloses calcium cantharidinate and a preparation method thereof. The structure formula of the calcium cantharidinate is shown in a formula (I). The preparation method comprises the following steps: adding trichloromethane or isopropanol in pure cantharidin in a weight ratio of 1: (30-50), and heating for dissolving pure cantharidin and simultaneously, adding calcium hydroxide intodistilled water of which the volume is same as that of trichloromethane or isopropanol to prepare a suspension, wherein the molar ratio of pure cantharidin to calcium hydroxide is 3:2; adding the calcium hydroxide suspension to the trichloromethane or isopropanol solution with dissolved cantharidin, heating to 60-75 DEG C, and then drying trichloromethane or isopropanol in a volatilizing manner so as to obtain a white suspension; concentrating the white suspension in a drying oven, and drying so as to obtain white crystal powder; and adding trichloromethane or isopropanol to the white crystalpowder in a weight ratio of 1: (30-50), heating to 40 DEG C, maintaining the temperature so as to dissolve the cantharidin, filtering, and drying so as to obtain white crystal powder which is the finished calcium cantharidinate. The finished calcium cantharidinate has high anticancer activity, stable property and high purity; and the preparation method is simple and is easy to operate and has good safety.

Description

technical field [0001] The invention belongs to the technical field of chemistry, in particular to calcium cantharidinate, and also to a preparation method of the calcium cantharidinate. Background technique [0002] In the first and second centuries, my country began to use mylabris to treat tumors. Later, it was confirmed that the cantharidin and cantharidin derivatives secreted by the cantharidin were the main effective substances. Because cantharidin is insoluble in water, it is often used as an oral drug application, which limits the application range of cantharidin. Later, people developed sodium cantharidinate to increase water solubility and reduce toxicity. Using this excellent property, developed a Cantharidin Sodium Injection can be injected directly. So far, Cantharidin Sodium Injection has been successfully applied clinically and achieved remarkable results. However, when the toxicity of sodium cantharidinate is reduced, the anticancer activity is greatly redu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/08A61P35/00
Inventor 李晓飞刘云娄方明时勇鹏陈永正
Owner ZUNYI MEDICAL UNIVERSITY