阅读说明：本技术 一种快速制取青蒿素的分离制备方法 (Separation preparation method for rapidly preparing artemisinin ) 是由 马峰 石学敏 马绍桓 梁秀红 于 2019-09-24 设计创作，主要内容包括：本发明提供一种快速制取青蒿素的分离制备方法,涉及青蒿素制备技术领域。该快速制取青蒿素的分离制备方法,包括以下步骤：1)脱水浸泡：选取若干原材料青蒿,将青蒿送入再脱水设备中进行脱水处理,脱水处理之后,将青蒿放入到双氧水中浸泡,然后取出青蒿用清水反复清洗2-4次,再利用脱水设备脱水,然后送入到干燥设备中做干燥处理；2)粉碎制粒：将步骤1中处理之后的青蒿用粉碎机进行粉碎处理,粉碎次数为3-5次,并将粉碎后的青蒿进行制粒,使得制成的青蒿颗粒粒度为10-15目。通过合理对原材料青蒿进行处理,使得青蒿在萃取过程中青蒿内部能够快速的与超临界二氧化碳接触,从而大大减少了萃取的时间,提高了青蒿素制备效率。(The invention provides a separation preparation method for rapidly preparing artemisinin, and relates to the technical field of artemisinin preparation. The separation preparation method for rapidly preparing the artemisinin comprises the following steps: 1) dewatering and soaking: selecting a plurality of raw materials, namely, sweet wormwood, feeding the sweet wormwood into secondary dehydration equipment for dehydration, after the dehydration, putting the sweet wormwood into hydrogen peroxide for soaking, taking out the sweet wormwood, repeatedly washing the sweet wormwood for 2-4 times by using clear water, dehydrating by using the dehydration equipment, and feeding the sweet wormwood into drying equipment for drying; 2) and (3) crushing and granulating: and (2) crushing the sweet wormwood herb treated in the step (1) by using a crusher for 3-5 times, and granulating the crushed sweet wormwood herb to ensure that the particle size of the prepared sweet wormwood herb is 10-15 meshes. Through reasonably processing the raw material, namely the sweet wormwood herb, the sweet wormwood herb can be quickly contacted with supercritical carbon dioxide in the extraction process, so that the extraction time is greatly shortened, and the preparation efficiency of the sweet wormwood herb is improved.)

1. A separation preparation method for rapidly preparing artemisinin is characterized in that: the method comprises the following steps:

1) dewatering and soaking: selecting a plurality of raw materials, namely, sweet wormwood, feeding the sweet wormwood into secondary dehydration equipment for dehydration, after the dehydration, putting the sweet wormwood into hydrogen peroxide for soaking, taking out the sweet wormwood, repeatedly washing the sweet wormwood for 2-4 times by using clear water, dehydrating by using the dehydration equipment, and feeding the sweet wormwood into drying equipment for drying;

2) and (3) crushing and granulating: crushing the sweet wormwood herb treated in the step 1 by using a crusher for 3-5 times, granulating the crushed sweet wormwood herb to enable the particle size of the prepared sweet wormwood herb particles to be 10-15 meshes, and storing the prepared sweet wormwood herb particles at 15-20 ℃ for later use;

3) and (3) sweet wormwood extraction: placing a plurality of sweet wormwood granules in an extraction kettle, then using a heating device and a pressurizing device to enable carbon dioxide to reach a critical state and pumping the carbon dioxide into the extraction kettle, introducing a proper amount of entrainer into the extraction kettle during extraction, simultaneously keeping the flow of the carbon dioxide at 12-20L/h during the extraction process, controlling the pressure in the extraction kettle at 25-40MPa, controlling the temperature in the extraction kettle at 45-75 ℃, and extracting for 1-2 hours;

4) separation: after extraction, adjusting the pressure of the extraction kettle, discharging carbon dioxide fluid, resolving and separating the carbon dioxide fluid through a separation device to obtain artemisinin, and simultaneously concentrating the artemisinin to obtain crude artemisinin;

5) purification and crystallization: adding ethanol solvent into the crude artemisinin, and purifying and crystallizing.

2. The separation and preparation method for rapidly preparing artemisinin according to claim 1, characterized in that: the purity of the carbon dioxide is more than 99%, the purity of the entrainer is more than 96%, and the concentration of the hydrogen peroxide is 0.2-0.3%.

3. The separation and preparation method for rapidly preparing artemisinin according to claim 1, characterized in that: the temperature is controlled within the range of 5-15 ℃ and the pressure is controlled within the range of 1-10MPa during separation.

4. The separation and preparation method for rapidly preparing artemisinin according to claim 1, characterized in that: the entrainer is one of ethanol, ether, methanol, sunflower seed oil and peanut oil, preferably ether, and the mass of the entrainer is 2-3% of that of the sweet wormwood in the extraction kettle.

Technical Field

The invention relates to the technical field of artemisinin preparation, in particular to a separation preparation method for quickly preparing artemisinin.

Background

The artemisinin is a sesquiterpene lactone drug extracted from plant artemisia apiacea and provided with a peroxy group, and has an influence on an ultramicro structure of a mouse plasmodium in the erythrocytic stage, mainly changes the structure of a plasmodium membrane system.

At present, the variety of the preparation methods of the artemisinin is more, and the preparation methods mainly comprise a chemical synthesis method, a biological synthesis method, an extraction method and the like, wherein a plurality of artemisinin is generally extracted by using supercritical carbon dioxide fluid, so that the extracted artemisinin is environment-friendly and harmless, but in the prior art, when the carbon dioxide fluid is used for extracting the artemisinin, the artemisinin extraction process is longer because the artemisia apiacea is not well pretreated before extraction, and the preparation efficiency of the artemisinin is reduced.

Disclosure of Invention

Technical problem to be solved

Aiming at the defects of the prior art, the invention provides a separation preparation method for rapidly preparing artemisinin, and solves the problems that the artemisinin extraction process is longer and the artemisinin preparation efficiency is reduced because the artemisia apiacea is not well pretreated before extraction when carbon dioxide fluid is used for extracting artemisinin in the prior art.

(II) technical scheme

In order to achieve the purpose, the invention is realized by the following technical scheme: a separation preparation method for rapidly preparing artemisinin comprises the following steps:

1) dewatering and soaking: selecting a plurality of raw materials, namely, sweet wormwood, feeding the sweet wormwood into secondary dehydration equipment for dehydration, after the dehydration, putting the sweet wormwood into hydrogen peroxide for soaking, taking out the sweet wormwood, repeatedly washing the sweet wormwood for 2-4 times by using clear water, dehydrating by using the dehydration equipment, and feeding the sweet wormwood into drying equipment for drying;

2) and (3) crushing and granulating: crushing the sweet wormwood herb treated in the step 1 by using a crusher for 3-5 times, granulating the crushed sweet wormwood herb to enable the particle size of the prepared sweet wormwood herb particles to be 10-15 meshes, and storing the prepared sweet wormwood herb particles at 15-20 ℃ for later use;

3) and (3) sweet wormwood extraction: placing a plurality of sweet wormwood granules in an extraction kettle, then using a heating device and a pressurizing device to enable carbon dioxide to reach a critical state and pumping the carbon dioxide into the extraction kettle, introducing a proper amount of entrainer into the extraction kettle during extraction, simultaneously keeping the flow of the carbon dioxide at 12-20L/h during the extraction process, controlling the pressure in the extraction kettle at 25-40MPa, controlling the temperature in the extraction kettle at 45-75 ℃, and extracting for 1-2 hours;

4) separation: after extraction, adjusting the pressure of the extraction kettle, discharging carbon dioxide fluid, resolving and separating the carbon dioxide fluid through a separation device to obtain artemisinin, and simultaneously concentrating the artemisinin to obtain crude artemisinin;

5) purification and crystallization: adding ethanol solvent into the crude artemisinin, and purifying and crystallizing.

Preferably, the purity of the carbon dioxide is more than 99%, the purity of the entrainer is more than 96%, and the concentration of the hydrogen peroxide is 0.2-0.3%.

Preferably, the temperature during the separation is controlled within the range of 5-15 ℃, and the pressure is controlled within the range of 1-10 MPa.

Preferably, the entrainer is one of ethanol, diethyl ether, methanol, sunflower seed oil and peanut oil, preferably diethyl ether, and the mass of the entrainer introduced is 2-3% of that of the sweet wormwood in the extraction kettle.

(III) advantageous effects

The invention provides a separation preparation method for quickly preparing artemisinin. The method has the following beneficial effects:

1. according to the separation preparation method for rapidly preparing the artemisinin, the raw material of the artemisia apiacea is reasonably treated, so that the interior of the artemisia apiacea can be rapidly contacted with the supercritical carbon dioxide in the extraction process, the extraction time is greatly shortened, and the artemisinin preparation efficiency is improved.

2. The separation preparation method for rapidly preparing the artemisinin ensures that the purity of the prepared artemisinin is better by reasonably introducing the entrainer.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to a plurality of embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.