Method for extracting mersosin by ultrasonic field assisted with mixed solvent

A technology of mixed solvent and extraction method, which is applied in the field of comprehensive extraction of azadirachtin, can solve the problems of slow extraction speed, low operating temperature, complex equipment, etc., and achieve the goal of increasing extraction rate, increasing production capacity, and increasing concentration gradient Effect

Inactive Publication Date: 2008-05-14
HEFEI UNIV OF TECH
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  • Abstract
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Problems solved by technology

Due to the medium polarity of azadirachtin and a lot of impurities in neem bark or seeds, it is difficult to extract them all by conventional solvent extraction, and the extraction speed is slow, the extraction efficiency is low, and the solvent consumption is too large
[0003] The supercritical carbon dioxide extraction method has good selectivity and low operating temperature. It is suitable for extracting heat-sensitive components that must be extracted at room temperature, but the extraction cost is high and the equipment is complicated. Substance is not appropriate
Microwave has a strong penetrating power. It can heat the inner and outer parts of the extract evenly and rapidly at the same time, so the efficiency of microwave-assisted extraction is high, but it is not suitable for the extraction of heat-sensitive components, and microwave extraction equipment is difficult to manufacture and difficult to realize. serial production
[0004] Existing at home and abroad utilize ultrasonic to assist the report of extracting azadirachtin (Azadirachtin) from another Meliaceae plant neem, as Chen Yuming mentioned in CN03117359.4 the comprehensive extraction method that solvent method is combined with ultrasonic wave, will The neem seeds after oil extraction were crushed and added to the extraction solvent, and ultrasonic waves were used to intensify the extraction treatment. The results proved that the extraction rate of azadirachtin increased from 65% to 75% in the single solvent method to 85% in 20 minutes of extraction. % or more, but this invention only comprehensively extracts neem kernels, the content of active ingredients in the kernels is relatively high, and the extraction is easy; on the one hand, taking bark or tree seeds as the extraction objects can reduce the work of raw material pretreatment On the one hand, because of the many impurities, it is difficult to achieve a good extraction effect
So far, there has been no report about the extraction of effective components of Meliaceae plants, especially the extraction of azadirachtin, by ultrasonic-assisted method and mixed solvent method.

Method used

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  • Method for extracting mersosin by ultrasonic field assisted with mixed solvent
  • Method for extracting mersosin by ultrasonic field assisted with mixed solvent

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Grind the dried neem bark to 60 mesh, put 10 grams in a 250mL flask, add 100mL of mixed solvent in a ratio of 1:10 and mix evenly, wherein the mixed solvent is prepared by mixing distilled water and ethanol analytical pure reagent , the volume concentration of ethanol in the mixed solvent is 70%, therefore, the polar parameter of the mixed solvent is 6.07, namely: ethanol 4.3×0.7+water 10.2×0.3, at ultrasonic frequency 40kHz, ultrasonic body power density 10W / L, leaching Extract at a temperature of 70°C for 40 minutes; after filtration, put the filter residue into a 250mL flask, add 100mL of the above mixed solvent again, and extract for 40 minutes at an ultrasonic frequency of 40kHz, an ultrasonic volume power density of 10W / L, and 70°C. After filtering, combine the filtrates, distill under reduced pressure, then add 50 mL of n-butanol to extract for 24 hours to obtain the extract, repeat 3 times, combine the extracts, evaporate and dry under reduced pressure to obtain ...

Embodiment 2

[0024] Grind the dried neem bark to 40 mesh, put 10 grams in a 250mL flask, add 150mL of mixed solvent in a ratio of 1:15 and mix evenly, wherein the mixed solvent is prepared by mixing distilled water and methanol analytical pure reagent , the volume concentration of methanol in the mixed solvent is 70%, therefore, the polar parameter of the mixed solvent is 7.68, namely: methanol 6.6×0.7+water 10.2×0.3, at ultrasonic frequency 45kHz, ultrasonic body power density 5W / L, leaching Extract at a temperature of 80°C for 30 minutes; after filtration, put the filter residue into a 250mL flask, add 150mL of the above mixed solvent, and extract again at an ultrasonic frequency of 45kHz, an ultrasonic volume power density of 5W / L, and 80°C for 30 minutes. After filtration, the filtrates were combined, distilled under reduced pressure, and then 50 mL of ethyl acetate was added to extract for 24 hours to obtain an extract. The extraction was repeated 3 times, and the extracts were combine...

Embodiment 3

[0026] Grind the dried neem seeds to 20 mesh, get 10 grams and place them in a 250mL flask, add 50mL of mixed solvent according to the ratio of 1:5 and mix evenly. The mixed solvent is analyzed by acetone and dichloromethane with a volume ratio of 1:1 Pure reagents are mixed and prepared. Therefore, the polarity parameter of the mixed solvent is 4.4, namely: acetone 5.4×0.5+dichloromethane 3.4×0.5, at an ultrasonic frequency of 100kHz, an ultrasonic volume power density of 20W / L, and an extraction temperature of 70°C , leaching for 40 minutes. After filtration, put the filter residue into a 250mL flask, add 50mL of the above-mentioned mixed solvent, and extract again at an ultrasonic frequency of 100kHz, an ultrasonic bulk power density of 20W / L, and 70°C for 40 minutes. After filtration, the filtrates were combined, distilled under reduced pressure, and then 50 mL of ethyl acetate was added to extract for 24 hours to obtain an extract, which was repeated 3 times. The extracts...

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Abstract

The invention relates to an ultrasonic field-assistant Toosendanin extraction method for compound solvent, which is characterized in that: the chopped Melia azedarach barks and seeds are directly used as the extraction object and are put into the extraction solvent; the extraction solvent with the extraction object is put into an ultrasonic field to obtain the powder with Toosendanin after distillation and concentration, extraction and separation and evaporation drying orderly; the extraction solvent is a compound solvent with solvents of two or more polarities. The invention has the advantages that: the cavitation effect, the thermal effect and the mechanical effect of ultrasonic wave are adopted in the process; the cell walls of the Melia azedarach barks or the seeds are effectively broken; the compound solvent regulates the polarity of the extract, enabling the effective components flow out of the cells into the solution body, and efficiently reducing the solvent consumption and the extraction cost.

Description

technical field [0001] The invention relates to an external field-assisted extraction process of natural products, in particular to a comprehensive extraction method for extracting azadirachtin assisted by an ultrasonic field. Background technique [0002] Toosendanin (toosendanin) is a tetracyclic triterpenoid extracted from the natural plant Neem or Toosendan. It has certain medical therapeutic effects, and has good broad-spectrum insecticidal and antibacterial properties. It is harmless to the human body, easy to degrade, and can It is a kind of botanical pesticide with great potential to prevent and control crop diseases and insect pests. The extraction methods of effective components of Meliaceae mainly include conventional solvent extraction, supercritical fluid extraction, microwave-assisted extraction and ultrasonic field-assisted extraction. Because azadirachtin has medium polarity and there are many impurities in neem bark or seeds,...

Claims

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Application Information

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IPC IPC(8): C07J71/00A61K36/58
Inventor 路绪旺崔鹏
Owner HEFEI UNIV OF TECH
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