CN100508995C - Method for processing lucid ganoderma spore oil preparations enriched with terpenes - Google Patents
Method for processing lucid ganoderma spore oil preparations enriched with terpenes Download PDFInfo
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- CN100508995C CN100508995C CNB2006100860751A CN200610086075A CN100508995C CN 100508995 C CN100508995 C CN 100508995C CN B2006100860751 A CNB2006100860751 A CN B2006100860751A CN 200610086075 A CN200610086075 A CN 200610086075A CN 100508995 C CN100508995 C CN 100508995C
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Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
本发明公开了一种富含萜类的灵芝孢子油类制剂加工方法。该方法是将经CO2超临界萃取得到的灵芝孢子油采用截留分子量为1000～2000道尔顿的超滤膜进行超滤分离，超滤分离时控制温度为30～40℃，压力为0.4～0.6MPa，超滤时间为2～4h，即可得到富含萜类的灵芝孢子油。该方法成本低，污染少，操作简单，易于产业化应用，能将灵芝孢子油中总三萜含量的纯度提高了近1倍左右，并且三萜类物质浓缩后的质量不受影响。The invention discloses a processing method of ganoderma lucidum spore oil preparation rich in terpenoids. The method is to separate the Ganoderma lucidum spore oil obtained by supercritical CO2 extraction with an ultrafiltration membrane with a molecular weight cut-off of 1000-2000 Daltons. During ultrafiltration, the temperature is controlled at 30-40°C and the pressure is 0.4-2000. 0.6MPa, and the ultrafiltration time is 2-4 hours, and the Ganoderma lucidum spore oil rich in terpenoids can be obtained. The method has the advantages of low cost, less pollution, simple operation, and easy industrial application, and can increase the purity of the total triterpene content in the ganoderma lucidum spore oil by about one time, and the quality of the concentrated triterpenoids is not affected.
Description
Technical field
The invention belongs to the Ganoderma manufacture field, relate to a kind of processing method that is rich in the Ganoderma spore oils preparation of terpenoid.
Background technology
Ganoderma is the treasure in the Chinese medicine and pharmacy treasure-house.Ancient oriental people, especially Chinese are described as " miraculous cure " that can come back to life to Ganoderma, can cure " Herba mesonae chinensis ", " Ganoderma " of all kinds of diseases and ailments, and are considered as its symbol for " having good luck ".In the Ancient Times in China document, the works of many Ganodermas of touching upon is arranged.Shennong's Herbal is included into Ganoderma top grade, promptly effective and nontoxic good medicine.The Compendium of Material Medica of Li Shizhen (1518-1593 A.D.) claim Ganoderma can " main deafness, sharp joint, protect the refreshing beneficial motive, invigorating middle warmer, increase wisdom, hard muscles and bones, good color ", " treat asthenia, control hemorrhoid ", clothes " make light of one's life by commiting suicide and do not prolong life always " for a long time.Ganoderma spore is the Ganoderma growth and maturity phase to eject ultrafine spore from cap, is the sexual cell of Ganoderma, has the whole hereditary active substance of Ganoderma.Contain protein and amino acids, glycopeptide class, vitamins, carotene, sterols, triterpenes, alkaloids, fatty acid, lactone and inorganic ions class etc. in the Ganoderma spore.
Modern study has confirmed that Ganoderma spore has antitumor, anticancer, immunomodulating, protects the liver, blood sugar lowering, anti-hypoxia, antiinflammatory, removing free radical and to functions such as neural regulating actions.It is main because it contains efficacy factor, especially triterpene substances such as ganoderan, triterpene substance that Ganoderma has above-mentioned effect, and it is having peculiar curative effect aspect anti-tumor, the hepatoprotective.
Antitumor action---there is research from Ganoderma spore, to extract and obtains 6 triterpenoid compound ganoderic acid U that cytotoxic activity is arranged, V, W, X, Y and Z, experiment in vitro show the propagation that can obviously suppress Mouse Liver sarcoma (HTC) cell.Other has the scholar to be separated to 2 triterpenoid compound ganoderal A and two hydrogen ganoderal A from Ganoderma spore, and experiment in vitro shows that both have stronger antitumor activity, to people's hepatosarcoma cell and KB cell ED
50Value is all at 1～11 μ gmL
-1, the strongest with ganoderal A effect.
Hepatoprotective effect---there is the scholar from the Ganoderma lucidum (Leyss. Ex Fr.) Karst. spore, to obtain thick component GT, further gets 5 components (GT1～GT5), detect this GT of confirmation and GT through HPLC through silica gel column chromatography
2Mainly contain Ganodenic acid A and Ganoderma lucidum (Leyss. Ex Fr.) Karst. acid A.Experiment shows GT and GT
23 kinds of liver injury model mices due to carbon tetrachloride, galactosaminide and the bacillus calmette-guerin vaccine+lipopolysaccharide are had hepatoprotective effect preferably, can obviously reduce Serum ALT and the liver TG content of animal pattern, and different degree alleviates the animal liver damage.In the test of mouse immune liver damage (BCG+LPS) primary hepatocyte In vitro culture, the author observes GT (0.5,5.0,50,100 μ gmL
-1) and GT2 (0.5,2.0,10,50 μ gmL
-1) can reduce the content of the active and NO of ALT in the damage hepatocyte supernatant to some extent, act on similar to positive control drug Malotilate (malotilate).
With supercritical CO
2Main functional component is exactly a triterpene substance in the Ganoderma spore oil that abstraction technique obtains, and its molecular weight is between 400～600.Remaining composition mainly exists with the form of triglyceride, as oleic acid, linoleic acid, Palmic acid etc., in addition, also contains small-amount free fatty acid and steroid ester, and the molecular weight of these materials is about about 1000～2000.
But, because industrial employing supercritical CO
2Total triterpene contents in the Ganoderma spore oil that abstraction technique obtains is not high, approximately have only about 20%, if directly take behind the preparation, then there is functional component content low, shortcomings such as dose is big, and taken in a large amount of oils and fatss virtually, human body has been increased suffer from obesity, hyperlipidemia, hypertensive risk.Therefore, need carry out enrichment method to the total triterpene in the Ganoderma spore oil handles.Original technology adopts adsorption resin method, promptly utilizes the loose structure and the selective absorption function of adsorbent resin, the triterpene substance in the Ganoderma spore oil is carried out separation and concentration concentrate.
This method shortcoming: commercially available adsorbent resin contains compositions such as unconverted monomer, cross-linking agent, dispersant and antiseptic more at present, and these organic substances may damage health after entering human body as medical material.In addition, the character of the triterpene substance of this method in also can Ganoderma spore changes to some extent.Therefore, need resin is carried out pretreatment, and formulate corresponding solvent method for detecting residue and rational content limit, to guarantee clinical safety.In addition, resin absorbability decline can occur after using repeatedly and resin is degraded, the situations such as processing of waste resin.
Membrane separation technique has efficiently, process does not have phase transformation, can operate at normal temperatures, technology is simple, easy to operate, advantages such as floor space is little, low pollution, become emerging being used to and the green energy conservation technology of aspect such as clarified, separated and concentrated, obtained application more and more widely in fields such as food, biological medicine, environmental protection, chemical industry.Still there is not at present the research report that this technology of employing concentrates total triterpene in the Ganoderma spore oil.
Summary of the invention
The purpose of this invention is to provide that a kind of cost is low, technology is simple, total spissated processing method of triterpene enrichment in the oligosaprobic Ganoderma spore oil.
The objective of the invention is to realize by following technical measures:
A kind of Ganoderma spore oils preparation processing method that is rich in terpenoid, this method will be through CO
2It is that 1000～2000 daltonian ultrafilter membranes carry out ultra-filtration and separation that the Ganoderma spore oil that supercritical extraction obtains adopts molecular cut off, can obtain being rich in the Ganoderma spore oil of terpenoid.Wherein ultra-filtration and separation time control temperature is 30～40 ℃, and pressure is 0.4～0.6MPa, and the ultrafiltration time is 2～4h.
Beneficial effect of the present invention:
The present invention utilizes membrane separation technique that the Ganoderma spore oil that adopts supercritical extraction is carried out concentration, the purity of total triterpene contents in the Ganoderma spore oil has been improved nearly about 1 times, reach 37%～39% (mass percent, down together), and the quality after triterpene substance concentrates is unaffected, can better play the effect that suppresses tumor and protect the liver.This method cost is low, pollutes and lacks, and is simple to operate, is easy to commercial application.
Adopt triterpenes content contrast in the isolating Ganoderma spore oil of membrane separating method provided by the invention and adsorption resin method institute:
The supercritical CO of learning from else's experience
2Extract the Ganoderma spore oil that obtains (wherein total triterpene contents is respectively: 20.4%, 22.5%, 19.8%), adopt conventional adsorption resin method to separate enrichment method respectively with membrane separating method provided by the invention (seeing embodiment for details), total triterpene concentration ratio sees Table 1 in the gained Ganoderma spore oil, and the content of gained Ganoderma spore well cuts (i.e. other compositions except that total triterpene, oils and fats) relatively sees Table 2.
Table 1:
| 1 | 2 | 3 | |
| Supercritical CO 2The concentration of total triterpene in the extraction gained Ganoderma spore oil | 20.4％ | 22.5％ | 19.8％ |
| Membrane separation process of the present invention is handled total triterpene concentration in the Ganoderma spore oil of back | 38.4％ | 39.2％ | 37.7％ |
| Adsorption resin method is handled total triterpene concentration in the Ganoderma spore oil of back | 35.1％ | 35.9％ | 34.4％ |
Table 2:
| 1 | 2 | 3 | |
| Supercritical CO 2Impurity content in the extraction gained Ganoderma spore oil | 0.12％ | 0.14％ | 0.15％ |
| Membrane separation process of the present invention is handled the impurity content in the Ganoderma spore oil of back | 0.11％ | 0.10％ | 0.12％ |
| Adsorption resin method is handled the impurity content in the Ganoderma spore oil of back | 0.21％ | 0.19％ | 0.18％ |
The specific embodiment
The invention will be further elaborated by the following examples.
General explanation:
Used in following examples through supercritical CO
2The Ganoderma spore oil that technology extraction obtains be adopt that the patent No. is 99123952.0, name is called the Ganoderma spore oil that the patent documentation disclosed method of " a kind of supercritical processing method of Ganoderma spore " prepares, concrete steps are: (1) adds the mixture of entry, gelatin, starch or wherein a kind of edible additive with Ganoderma spore powder, addition is as the criterion the Ganoderma spore powder molding bonded, mix homogeneously, extrusion modling at room temperature, natural drying; (2) during the Ganoderma spore powder of dry aftershaping is packed extractor into, feed CO from the extractor bottom
2Gas, the control temperature is 35～65 ℃, and pressure is 20～35MPa, and the extraction time is 1～35 hour; (3) flow out the CO that contains Ganoderma spore oil from extractor top
2Enter the decompression separation device, Ganoderma spore oil is emitted CO from decompression separation device bottom
2Gas flows out from the top of decompression separation device; (4) it is standby the water in the Ganoderma spore oil and jelly to be separated the Ganoderma spore oil that obtains purification after removing, and reclaims the defat Ganoderma spore powder from extractor.
The Ganoderma spore oil that is used for the total triterpene of membrane separation process enrichment of the present invention also can adopt other supercritical COs
2The Ganoderma spore oil that the technology extraction obtains.
Supercritical CO
2The Ganoderma spore oil that the technology extraction obtains mainly is made up of three parts: total triterpene (being functional component), impurity, oils and fats (being solvent).
Purity in the Ganoderma spore oil of high-purity described in the embodiment=(total triterpene+oils and fats)/(total triterpene+impurity+oils and fats) * 100%.
Embodiment 1
To adopt supercritical CO
2After water in the Ganoderma spore oil that the technology extraction obtains and jelly separation are removed, collect highly purified Ganoderma spore oil (wherein total triterpene contents is 21.8%, impurity content 0.17%).The Ganoderma spore oil that collection is obtained adds in the material liquid storage tank of membrane separation plant, the control temperature is carried out ultra-filtration and separation at 30～40 ℃, and it is 1000～2000 daltonian polyamide rolled films that ultrafilter membrane adopts molecular cut off, pressure is controlled at 0.4～0.6MPa, ultrafiltration time 2～4h.To finally collecting, obtain total triterpene contents and reach 38.1% Ganoderma spore oil by the feed liquid of ultrafilter membrane.
Embodiment 2
To adopt supercritical CO
2After water in the Ganoderma spore oil that the technology extraction obtains and jelly separation are removed, collect highly purified Ganoderma spore oil (wherein total triterpene contents is 20.4%, impurity content 0.12%).The Ganoderma spore oil that collection is obtained adds in the material liquid storage tank of membrane separation plant, the control temperature is carried out ultra-filtration and separation at 30～40 ℃, and it is 1000～2000 daltonian polyamide rolled films that ultrafilter membrane adopts molecular cut off, pressure is controlled at 0.4～0.6MPa, control time 3.5h.To finally collecting, obtain total triterpene contents and reach 38.4% Ganoderma spore oil by the feed liquid of ultrafilter membrane.
Embodiment 3
To adopt supercritical CO
2After water in the Ganoderma spore oil that the technology extraction obtains and jelly separation are removed, collect highly purified Ganoderma spore oil (wherein total triterpene contents is 22.5%, impurity content 0.14%).The Ganoderma spore oil that collection is obtained adds in the material liquid storage tank of membrane separation plant, the control temperature is carried out ultra-filtration and separation at 30～40 ℃, and it is 1000～2000 daltonian polyamide rolled films that ultrafilter membrane adopts molecular cut off, pressure is controlled at 0.4～0.6MPa, control time 3.5h.To finally collecting, obtain total triterpene contents and reach 39.2% Ganoderma spore oil by the feed liquid of ultrafilter membrane.
Embodiment 4
To adopt supercritical CO
2After water in the Ganoderma spore oil that the technology extraction obtains and jelly separation are removed, collect highly purified Ganoderma spore oil (wherein total triterpene contents is 19.8%, impurity content 0.15%).The Ganoderma spore oil that collection is obtained adds in the material liquid storage tank of membrane separation plant, the control temperature is carried out ultra-filtration and separation at 30～40 ℃, and it is 1000～2000 daltonian polyamide rolled films that ultrafilter membrane adopts molecular cut off, pressure is controlled at 0.4～0.6MPa, control time 3.5h.To finally collecting, obtain total triterpene contents and reach 37.7% Ganoderma spore oil by the feed liquid of ultrafilter membrane.
Claims (1)
1, a kind of Ganoderma spore oils preparation processing method that is rich in terpenoid is characterized in that through CO
2It is that 1000～2000 daltonian ultrafilter membranes carry out ultra-filtration and separation that the Ganoderma spore oil that supercritical extraction obtains adopts molecular cut off, the control temperature is 30～40 ℃ during ultra-filtration and separation, pressure is 0.4～0.6MPa, and the ultrafiltration time is 2～4h, can obtain being rich in the Ganoderma spore oil of terpenoid.
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| 灵芝多糖与三萜类的提取纯化工艺研究进展. 黄小琴等.食用菌学报，第12卷第3期. 2005 * |
| 现代实用中药新剂型新技术. 董方言，52，53，人民卫生出版社. 2001 * |
| 超滤膜分离技术在中药生产中的应用研究. 宁慧青.山西化工，第23卷第3期. 2003 * |
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