CN110790745A - A kind of preparation method of extracting vitacoxib from waste tablets - Google Patents

Abstract

The invention relates to a preparation method for extracting vitacoxib from waste tablets. Firstly, putting the waste vitamin tremble tablet powder which is crushed and sieved by a 60-mesh sieve into a dry reaction bottle, then putting an extraction solvent, filtering after the reaction is finished, heating the filtrate to evaporate the solvent, then adding purified water into the residue, stirring and filtering, washing a filter cake with purified water, drying in an oven, crushing and sieving by the 60-mesh sieve to obtain a pure product of the extracted vitamin tremble raw material medicament, wherein the extraction yield is more than 80 percent, and the content is more than 98.5 percent. The method has the advantages of simple and easily-controlled operation, high yield and low cost, and provides a new method for extracting raw medicines of the vitacoxib from the waste tablets of the vitacoxib.

Description

A kind of preparation method of extracting vitacoxib from waste tablets

technical field

The invention relates to a preparation method of medicinal chemicals, in particular to a preparation method of extracting vitacoxib from waste tablets.

Background technique

Vitacoxib is a new type of non-steroidal anti-inflammatory drug. Non-steroidal anti-inflammatory drugs can inhibit COX-2, thereby reducing the synthesis of various inflammatory mediators such as prostaglandins and thromboxane, thereby antipyretic and analgesic. , anti-inflammatory effect. Vitacoxib is suitable for pets to relieve pain and inflammation caused by osteoarthritis, and can be used for perioperative management of bone or soft tissue. Due to the influence of various factors in the early research and production process of Vitacoxib chewable tablets, unqualified tablets or tablets with expired validity period, also known as waste tablets, appear due to the synthesis process of Vitacoxib raw materials Complex, resulting in a higher price of Vitacoxib. If qualified vitaoxib can be extracted from these waste tablets, not only can the extracted vitaoxib be used reasonably, the production cost can be reduced, but also the burden of the three wastes treatment can be reduced, which is beneficial to the protection of the environment. In addition to the main drug Vitacoxib, the other excipients contained in Vitacoxib Chewable Tablets are lactose, microcrystalline cellulose, polyvinylpyrrolidone K30, sodium lauryl sulfate, sodium carboxymethyl starch and magnesium stearate . The composition of the vitacoxib chewable tablet is complex, the content of vitacoxib is low, and the content of each tablet is only 6%. How to find an effective extraction process is the problem to be solved by the present invention.

In the process of the present invention, in order to find a preparation method that can effectively extract vitacoxib, we firstly study the properties of the ingredients that make up the vitacoxib chewable tablet. After the analysis of the excipients in the tablet formulation and repeated preliminary experiments, the extraction solvent and extraction method were finally determined. The used extraction solvent can be reused repeatedly after recovery, which effectively reduces the extraction cost.

SUMMARY OF THE INVENTION

The purpose of the present invention is to provide a preparation method for extracting vitacoxib from waste tablets. provides a new approach.

To achieve the above object, the present invention adopts the following technical solutions:

First, put the vitacoxib waste tablet powder that has been pulverized through a 60-mesh sieve into a dry reaction bottle, then add an extraction solvent, control the extraction temperature and extraction time, and filter the filtrate after heating to evaporate the extraction solvent. , then add a crystallization solvent to the residue, filter after stirring, wash the filter cake with purified water, dry in an oven and pulverize it through a 60-mesh sieve to obtain the pure vitacoxib raw material drug, with an extraction yield of more than 80% , the content reaches more than 98.5%.

The extraction solvent is a mixed solvent of one or any combination of dichloromethane, ethyl acetate, chloroform and ethyl formate, and the preferred extraction solvent is ethyl acetate.

The extraction temperature is 20-25°C.

The extraction time is 30-60 minutes.

The crystallization solvent is purified water.

The preparation method of extracting vitacoxib from waste tablets of the present invention, more specifically, comprises the following steps:

First, put the vitacoxib waste tablet powder that has been crushed through a 60-mesh sieve into a dry reaction bottle, then add ethyl acetate, control the extraction temperature to be 20-25°C, and the extraction time to be 30-60 minutes, and the extraction reaction is completed. , filter, heat the filtrate to evaporate the ethyl acetate, then add purified water to the residue, filter after stirring, wash the filter cake with purified water, dry in an oven, pulverize and pass through a 60-mesh sieve to obtain the extracted vitacoxib The pure product of the raw material drug, the extraction yield is above 80%, and the content is above 98.5%.

The method is simple and easy to control, has high yield and low cost, and provides a new method for extracting the raw material medicine of vitacoxib from waste vitacoxib tablets.

Detailed ways

The following are the embodiments of the present invention, which are only used to illustrate the present invention, and should not be regarded as a limitation of the present invention.

Example 1

First, put 10 g of vitacoxib waste tablet powder that has been crushed through a 60-mesh sieve into a dry reaction bottle, then add 30 ml of dichloromethane, start stirring, control the extraction temperature at 20 °C, and stir and extract for 30 minutes, and the extraction reaction is completed. , filter with a Bush funnel, heat the filtrate to evaporate the dichloromethane, then add 10 ml of purified water to the residue, filter after stirring, wash the filter cake with purified water, pulverize the filtrate and pass through a 60-mesh sieve after drying in an oven to obtain the extracted The pure product of the raw material drug of Vitacoxib is 0.53g, the extraction yield is 88.3%, and the content is 98.7%.

Example 2

First, put 20 g of vitacoxib waste tablet powder that has been crushed through a 60-mesh sieve into a dry reaction bottle, then add 50 ml of ethyl acetate, start stirring, control the extraction temperature at 30 ° C, and stir and extract for 45 minutes, and the extraction reaction is completed. , filter with Bush funnel, heat the filtrate to evaporate ethyl acetate, then add 20 ml of purified water to the residue, filter after stirring, wash the filter cake with purified water, dry in an oven, pulverize and pass through a 60-mesh sieve to obtain the extracted 1.02g of pure vitacoxib raw material drug, the extraction yield is 85.0%, and the content is 99.1%.

The preparation method for extracting vitacoxib from waste tablets provided by the present invention has been described in detail above. In this paper, specific cases are used to illustrate the principles and implementations of the present invention. The descriptions of the above examples are only used to help understanding The method of the present invention and its core idea; at the same time, for those skilled in the art, according to the idea of the present invention, there will be changes in the specific implementation and application scope. In summary, the content of this specification should not be It is understood as a limitation of the present invention.

Claims (6)

1. a preparation method of extracting vitacoxib from waste tablets, is characterized in that, comprises the following steps: at first in a dry reaction flask, drop into the vitacoxib waste tablet powder that has been pulverized through 60 mesh sieves, then Add the extraction solvent, control the extraction temperature and extraction time, after the extraction reaction is completed, carry out filtration, heat the filtrate to evaporate the extraction solvent, then add crystallization solvent to the residue, filter after stirring, wash the filter cake with purified water, and dry it in an oven. Pulverized through a 60-mesh sieve to obtain the pure vitacoxib raw material drug, the extraction yield is over 80%, and the content reaches over 98.5%. 2. the preparation method of extracting vitacoxib from waste sheet as claimed in claim 1, is characterized in that, described extraction solvent is one of wherein dichloromethane, ethyl acetate, chloroform, ethyl formate One or any combination of mixed solvents, the preferred extraction solvent is ethyl acetate. 3 . The preparation method for extracting vitacoxib from waste tablets as claimed in claim 1 , wherein the extraction temperature is 20-25° C. 4 . 4. The preparation method of extracting vitacoxib from waste tablets as claimed in claim 1, wherein the extraction time is 30-60 minutes. 5. The preparation method of extracting vitacoxib from waste tablets as claimed in claim 1, wherein the crystallization solvent is purified water. 6. the preparation method of extracting vitacoxib from waste sheet as claimed in claim 1, is characterized in that, comprises the following steps: First, put the vitacoxib waste tablet powder that has been crushed through a 60-mesh sieve into a dry reaction bottle, then add ethyl acetate, control the extraction temperature to be 20-25°C, and the extraction time to be 30-60 minutes, and the extraction reaction is completed. , filter, heat the filtrate to evaporate the ethyl acetate, then add purified water to the residue, filter after stirring, wash the filter cake with purified water, dry in an oven, pulverize and pass through a 60-mesh sieve to obtain the extracted vitacoxib The pure product of the raw material drug, the extraction yield is above 80%, and the content is above 98.5%; The method is simple and easy to control, has high yield and low cost, and provides a new method for extracting the raw material medicine of vitacoxib from waste vitacoxib tablets.