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Method for separating camptothecin

A separation method and technology for camptothecin, applied in organic chemistry and other directions, can solve the problems of large solvent consumption, lower product price, and impact on product quality, etc., and achieve the effects of stable process, shortened working hours, and low cost.

Active Publication Date: 2014-09-03
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In general, the traditional extraction and separation method of camptotheca alkaloids has large solvent consumption, complex operation process, long duration, low extraction purity and high production cost
In addition, although the content of monomer impurities is already very low, it still seriously affects the quality of the product and greatly reduces the price of the product

Method used

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  • Method for separating camptothecin
  • Method for separating camptothecin
  • Method for separating camptothecin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take by weighing 10 grams of camptothecin extract (commercially available, Shanghai Kangting Biotechnology Co., Ltd.) (camptothecin content 50wt%, detected by liquid chromatography / LC-20AT Shimadzu liquid chromatograph, the calculated molar weight is 0.0144mol ), add 20mL of ethanol, stir evenly to obtain a suspension. Then suspension and active agent dedecyl guanidine (8 grams) are dropped into foam separation tower (Terada Pump Terada Pump Manufacturing Institute MS-S small foam separator, total capacity 2L, and the column height of foam separation tower and internal diameter ratio are 14: 1, the same below), the column height to inner diameter ratio of the foam separation tower is 14:1, the temperature in the foam separation tower is controlled at 30°C, the raw material liquid obtained by mixing the suspension and dedecylguanidine is stirred evenly, and passed through the tower Introduce air at the bottom, and the gas flow rate of the air is 12mL / min for bubbling, an...

Embodiment 2

[0032] Take by weighing camptotheca extractum (commercially available, Shanghai Kangting Biotechnology Co., Ltd.) 12 grams (camptothecin content 54%, liquid chromatography / LC-20AT Shimadzu liquid chromatograph detection, calculated molar weight is 0.0186mol ), add 25mL ethanol, stir evenly to obtain a suspension. Then suspension and active agent dodecyl guanidine (9 grams) are dropped in the foam separation tower, the temperature in the control foam separation tower is 30 ℃, the raw material liquid that suspension liquid and dodecyl guanidine are mixed gained is stirred, Air is introduced through the bottom of the tower with a gas flow rate of 15mL / min for bubbling, and the foam obtained is discharged from the top of the tower into a storage tank to obtain a foam liquid, and the foam is collected until no foam is produced. Centrifuge the resulting foam liquid at 10,000rpm for 20 minutes, take the centrifuged precipitate, put it into 18mL of 10wt% hydrochloric acid and stir it ...

Embodiment 3

[0034] Take by weighing camptotheca extractum (commercially available, Shanghai Kangting Biotechnology Co., Ltd.) 14 grams (camptothecin content 58%, liquid chromatography / LC-20AT Shimadzu liquid chromatograph detection, calculated molar weight is 0.0233mol ), adding 28mL of ethanol, under the condition of stirring, a suspension was obtained. The suspension is then mixed with the active agent cetylguanidine ( 15 g) into the foam separation tower, control the temperature in the foam separation tower to be 30°C, stir the raw material liquid obtained by mixing the suspension and cetylguanidine, introduce air through the bottom of the tower, and the gas flow rate of the air is 15mL / min , carry out bubbling, and the obtained foam is discharged into the storage tank from the top of the tower to obtain a foam liquid, and the foam is collected until no foam is produced. Centrifuge the foam liquid, centrifuge at 10000rpm for 25 minutes, take the centrifuged precipitate, then put the r...

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Abstract

The invention discloses a method for separating camptothecin, which comprises the following steps: mixing a camptotheca acuminate extract and ethanol, stirring to obtain a fluid suspension, then adding the obtained fluid suspension and a long chain guanidine radicals compound in a foam separating tower, continuously blowing air from the bottom of the foam separating tower to form foam, collecting the foam until no foam is generated, discharging the obtained foam from the top of the foam separating tower to obtain a foam liquid, centrifuging the obtained foam liquid, taking the centrifugation sediment, adding into an aqueous solution of inorganic acid, stirring for reacting to precipitate camptothecin, filtering, taking a filter cake, and drying to obtain the camptothecin finished product. The method has the advantages of low time consumption, low labor consumption, low cost, stable technology, low energy consumption, environmental protection and easy industrialization.

Description

(1) Technical field [0001] The invention relates to a method for separating camptothecin, in particular to a method for separating camptothecin by foam separation. (2) Background technology [0002] Camptothecin, a quinoline alkaloid, is the only inhibitor of topoisomerase I discovered so far, and it is also an effective anticancer agent. Because the content of camptothecin in amptothecin fruit is very low, about a few tenths to ten thousandths, and the harvesting of amptothecin is limited by seasons and regions, the production of camptothecin has been limited for many years. And the production cost is high, and the supply is in short supply at home and abroad. [0003] At present, the commonly used methods for separating camptotheca alkaloids include recrystallization, chromatography and chromatography, macroporous adsorption resin extraction, polyamide separation and purification, high-speed countercurrent chromatography separation, supercritical fluid CO 2 Extraction me...

Claims

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Application Information

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IPC IPC(8): C07D491/22
CPCC07D491/22
Inventor 王燕苗永夏春年金志敏
Owner ZHEJIANG UNIV OF TECH