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Method for extracting and separating thebaine from pericarpium papaveris

A technology of poppy husk and thebaine, which is applied in the field of plant extraction and purification, can solve the problems of low production efficiency of thebaine, difficulty in realizing poppy husk, and high fixed cost, and achieve easy construction, high yield, and low equipment investment. small effect

Active Publication Date: 2019-12-27
甘肃农垦药物碱厂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has relatively obvious disadvantages: (1) the high-pressure preparation and separation equipment used in it has huge fixed investment, and for large-scale production enterprises, the fixed cost has been raised invisibly; (2) the solution used must have a relatively high concentration, such as The minimum concentration of the upper column liquid indicated in the patent is about 35g / L, which is difficult to realize in the extraction of poppy shells; (3) because this method is not mainly used to separate thebaine, the yield is low, only about 73%; (4) pedicles The production efficiency of baine is low, so it is not suitable for industrial scale-up

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1 A method for extracting and separating thebaine from poppy shells, comprising the following steps:

[0031] (1) Add 3000 mL of acetic acid solution with a volume concentration of 0.5% to 500 g of poppy shells with a thebaine content of 2.1%, extract at a temperature of 55°C, and extract 6 times for 1.0 h each time to obtain an extract. The extraction residue was taken for detection, and the residue of thebaine in the detection of the extraction residue was 0.05%.

[0032] (2) After filtering the extract, put it on D101 resin (400mL) for adsorption, control the temperature at 20-40°C, flow rate at 0.5BV / h, and complete column loading; at 20-40°C and flow rate of 0.5BV / h, use 800mL resin to soften Wash the resin column with water, wash the resin column with 2400mL sodium hydroxide solution with a volume concentration of 1%, wash the resin column with 3200mL ethanol solution with a volume concentration of 20%, and then use 2400mL ethanol with a volume concentr...

Embodiment 2

[0036] Embodiment 2 A method for extracting and separating thebaine from poppy shells, comprising the following steps:

[0037] (1) Add 3000 mL of acetic acid solution with a volume concentration of 0.5% to 500 g of poppy shells with a thebaine content of 2.1%, extract at a temperature of 45°C, and extract 6 times for 1.0 h each time to obtain an extract. The extraction residue was taken for detection, and the residue of thebaine in the detection of the extraction residue was 0.05%.

[0038] (2) After the extract is filtered, apply D101 resin (400mL) for adsorption, control the temperature at 20-40°C, flow rate at 2.5BV / h, and complete column loading; at 20-40°C and flow rate of 2.0BV / h, use 1600mL resin to soften Wash the resin column with water, wash the resin column with 3200mL sodium hydroxide solution with a volume concentration of 1%, wash the resin column with 4000mL ethanol solution with a volume concentration of 20%, and then use 4800mL ethanol with a volume concentra...

Embodiment 3

[0042] Embodiment 3 A method for extracting and separating thebaine from poppy shells, comprising the following steps:

[0043] (1) Add 3000mL of acetic acid solution with a volume concentration of 0.5% to 500g of poppy shells with a thebaine content of 2.1%, the extraction temperature is 30°C, and the number of extractions is 6 times, each time 1.0h, to obtain an extract. The extraction residue was taken for detection, and the residue of thebaine in the detection of the extraction residue was 0.05%.

[0044](2) After the extract is filtered, apply D101 resin (400mL) for adsorption, control the temperature at 20-40°C, flow rate at 2.5BV / h, and complete column loading; at 20-40°C and flow rate of 2.0BV / h, use 1600mL resin to soften Wash the resin column with water, wash the resin column with 3200mL sodium hydroxide solution with a volume concentration of 1%, wash the resin column with 4000mL ethanol solution with a volume concentration of 20%, and then use 4800mL ethanol with a...

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Abstract

The invention relates to a method for extracting and separating thebaine from pericarpium papaveris, which comprises the following steps: (1) extracting or leaching pericarpium papaveris, of which thethebaine content is greater than 1% by using 0.5% acetic acid solution by a leakage method to obtain an extracting solution; (2) adsorbing and enriching the extracting solution by using macroporous resin or anion resin, and performing elution and desorption to obtain a desorption solution; (3) concentrating the desorption solution to be thick, adding a sodium hydroxide solution with the volume concentration of more than 20%, carrying out alkaline boiling, cooling the mixture to room temperature, and filtering the mixture to obtain a thebaine solid; (4) dissolving the thebaine solid in an acidsolution, adjusting the pH value with a 30% sodium hydroxide solution, crystallizing, filtering, and drying the filter cake to constant weight to obtain crude thebaine; and (5) crystallizing the crude thebaine with 95% ethanol to obtain a thebaine alkali product. The method is small in investment, high in yield and safe.

Description

technical field [0001] The invention relates to the field of plant extraction and purification, in particular to a method for extracting and separating thebaine from poppy shells. Background technique [0002] According to "Flora of China", opium poppy is specifically referred to as opium poppy. Poppy is the main raw material for producing opium, and its extract is also the source of various sedatives, such as morphine, thebaine, codeine, papaverine, and narcotine. The scientific name "somniferum" means "hypnotic", reflecting its narcotic properties. The main active ingredients in poppy are morphine, thebaine and narcotine. [0003] Thebaine is flaky crystal in ethanol, melting point is 193°C, specific optical rotation [α] is -218.5° (ethanol), -229° (chloroform), soluble in benzene, chloroform, pyridine, ethanol, slightly soluble in ether , Petroleum ether, almost insoluble in water. When thebaine encounters concentrated sulfuric acid, it turns blood red first, then turn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D489/02
CPCC07D489/02
Inventor 宋小兰王世余王邦荣祝可锦金鑫赵世本王丽萍常立昕陈双明王首太景艳顾秀芬张学松孔维申薛建宁
Owner 甘肃农垦药物碱厂有限公司
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