Method for preparing emodin and physcion from cassia seeds

A technology of emodin methyl ether and cassia seed, applied in organic chemistry, quinone separation/purification, etc., can solve the problems of low yield of extraction and purification, influence of active ingredients, loss of yield activity, etc., to save energy and time, and improve yield High, the effect of avoiding environmental pollution

Inactive Publication Date: 2019-01-15
西安绿海生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are several problems in the extraction and purification of emodin and emodin methyl ether: the extraction and purification yield of emodin and emodin methyl ether is very low; the use of a large amount of organic solvents (such as formic acid, ethyl formate, etc.) is easy to cause environmental pollution. Pollution and cost increase; the active ingredient is seriously affected by the extraction and purification process, and the increase in yield usually results in a loss of activity

Method used

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  • Method for preparing emodin and physcion from cassia seeds
  • Method for preparing emodin and physcion from cassia seeds
  • Method for preparing emodin and physcion from cassia seeds

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Effect test

Embodiment 1

[0024] A method for preparing emodin and emodin methyl ether from cassia seed, specifically comprising the following steps:

[0025] Weigh an appropriate amount of dried cassia seed, according to the conditions of 70% ethanol and cassia seed liquid ratio (g / mL) of 1:8, voltage 120V, rotating speed 3600r / min, at room temperature, after flash extraction for 60s, eight layers of gauze Filtrate, extract the residue repeatedly 3 times, and finally combine the extract; mix the crude extract with petroleum ether with a mass concentration of 60% according to the ratio of 1:15, shake for 24 hours, centrifuge, remove the residue and retain the liquid; take the pretreated crude The extract is added to the ultrafiltration material tank, and the transmembrane pressure difference and membrane surface flow rate are controlled by changing the pump speed and adjusting the sample outlet switch; the operating process temperature is 50°C, the transmembrane pressure difference is 0.3MPa, and the me...

Embodiment 2

[0027] A method for preparing emodin and emodin methyl ether from cassia seed, specifically comprising the following steps:

[0028] Cassia seed materials were selected from Fucheng District, Mianyang, Sichuan; JHBE-50S flash extractor; 19-channel ceramic membrane tube (support body ɑ-Al2O3, molecular weight cut-off 0.45 μm, effective membrane area 0.1m 2 ), CXUF-1X-500-19K ceramic membrane ultrafiltration experimental equipment; ZK-82B electric vacuum drying oven.

[0029] Weigh an appropriate amount of dried cassia seed, according to the conditions of 60% ethanol and cassia seed liquid ratio (g / mL) of 1:6, voltage 60V, rotating speed 3600r / min, at room temperature, after flash extraction for 120s, eight layers of gauze Filtrate, extract the residue repeatedly 3 times, and finally combine the extract; mix the crude extract with petroleum ether with a mass concentration of 60% according to the ratio of 1:15, shake for 24 hours, centrifuge, remove the residue and retain the liq...

Embodiment 3

[0031] A method for preparing emodin and emodin methyl ether from cassia seed, specifically comprising the following steps:

[0032] Cassia seed materials were selected from Fucheng District, Mianyang, Sichuan; JHBE-50S flash extractor; 19-channel ceramic membrane tube (support body ɑ-Al2O3, molecular weight cut-off 0.45 μm, effective membrane area 0.1m 2 ), CXUF-1X-500-19K ceramic membrane ultrafiltration experimental equipment; ZK-82B electric vacuum drying oven.

[0033] Weigh an appropriate amount of dried cassia seed, according to the conditions of 80% ethanol and cassia seed liquid ratio (g / mL) of 1:10, voltage 140V, rotating speed 3600r / min, at room temperature, carry out 90s flash extraction, eight layers of gauze Filtrate, extract the residue repeatedly 3 times, and finally combine the extract; mix the crude extract with petroleum ether with a mass concentration of 60% according to the ratio of 1:15, shake for 24 hours, centrifuge, remove the residue and retain the li...

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Abstract

The invention discloses a method for preparing emodin and physcion from cassia seeds, belonging to the field of functional component extraction. The method comprises the following steps: selecting dried leguminous cassia seeds for subsequent usage; weighing the dried cassia seeds, allowing a material-liquid ratio (g / mL) of the cassia seeds to 60-80% ethanol to be 1: (6-10), performing flash extraction under the condition of room temperature, a voltage of 60-140 V and a rotation speed of 3600 r / min for 60-120 s, then carrying out filtering with eight layers of gauze, repeatedly extracting residues three times, and finally combining obtained extracts; mixing a crude extract with a developing agent, carrying out vibrating and centrifugation, and removing residues while leaving liquid; clarifying, filtering and concentrating the obtained material by using a ceramic ultrafiltration membrane; and concentrating remaining aqueous-phase materials, adding the concentrated aqueous-phase materialsto excess ethanol for precipitation, and performing suction filtration to obtain emodin and physcion crystals. Compared with conventional processes, the method of the invention prevents heat-sensitive anthraquinone glycoside in Chinese rhubarb from thermal damage; and the flash extraction process is stable, rapid and highly-efficient, does not need heating, only takes 60 s in single extraction, and can save a great amount of energy and time when applied to industrial production.

Description

technical field [0001] The invention relates to the field of extraction of functional components, in particular to a method for preparing emodin and emodin methyl ether from cassia seeds. Background technique [0002] Semen Cassiae is the dry mature seed of the annual herbaceous plant Cassia officinalis or Cassia officinalis, also known as "Huantongzi". Semen Cassiae contains multiple vitamins and rich amino acids, fats, carbohydrates, etc. In recent years, its health care function has been paid more and more attention by people. Cassia seed has the functions of clearing liver-fire, dispelling rheumatism, benefiting kidney and improving eyesight, etc. Drinking cassia seed tea regularly can make blood pressure normal, defecate unobstructed, and prevent old eyes from blurring. Tobacco is an important economic crop in my country, but tobacco diseases, especially leaf diseases, are often prevalent and cause heavy losses. Emodin, the active ingredient in Semen Cassiae, is widel...

Claims

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Application Information

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IPC IPC(8): C07C50/34C07C46/10
CPCC07C46/10C07C50/34
Inventor 韩迎国安德荣崔秀坤程睿君安航
Owner 西安绿海生物科技有限公司
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