CN101450089B - Preparation method of mangrove extract liquid - Google Patents
Preparation method of mangrove extract liquid Download PDFInfo
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- CN101450089B CN101450089B CN2008102047365A CN200810204736A CN101450089B CN 101450089 B CN101450089 B CN 101450089B CN 2008102047365 A CN2008102047365 A CN 2008102047365A CN 200810204736 A CN200810204736 A CN 200810204736A CN 101450089 B CN101450089 B CN 101450089B
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- 235000020095 red wine Nutrition 0.000 claims description 3
- DGDGISHVMVMEBQ-IHXHSXLNSA-N (4ar,4bs,7s,8as,10as)-7-ethenyl-3-hydroxy-4b,7,10a-trimethyl-1-methylidene-5,6,8,8a,9,10-hexahydro-4ah-phenanthren-2-one Chemical compound C1=C(O)C(=O)C(=C)[C@]2(C)[C@H]1[C@@]1(C)CC[C@@](C=C)(C)C[C@@H]1CC2 DGDGISHVMVMEBQ-IHXHSXLNSA-N 0.000 abstract description 13
- DGDGISHVMVMEBQ-UHFFFAOYSA-N Tagalsin C Natural products C1=C(O)C(=O)C(=C)C2(C)C1C1(C)CCC(C=C)(C)CC1CC2 DGDGISHVMVMEBQ-UHFFFAOYSA-N 0.000 abstract description 13
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- Medicines Containing Plant Substances (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention discloses a method for preparing diterpene compound Tagalsin C in mangrove plants, which uses the root, stem, leaf and branch of mangrove plants as raw material, and performs complex enzyme treatment, 95% ethanol elution, ultrasonic auxiliary extraction and concentration to obtain Tagalsin C mangrove extracting solution.
Description
[technical field]
The present invention relates to the Chinese medicine extraction technical field.More specifically, the present invention relates to a kind of Rhizophora apiculata Blume extracting solution, also relate to the extracting solution method for preparing that contains new diterpene-kind compound Tagalsin C.
[background technology]
In the world, Rhizophora apiculata Blume has 84 kinds, is under the jurisdiction of 16 sections 24 and belongs to; Mainly be grown between south, the tropic of cancer, and can be divided into two crowd systems, promptly east crowd system (mainly is grown in Tropical Asia and Africa; There are 74 kinds; Being under the jurisdiction of 14 sections 18 belongs to) and west crowd system (mainly be grown in tropical America, have 10 kinds, be under the jurisdiction of 5 sections 6 and belong to).
China's ocean among the people medication such as mangrove plant have multiple disease treatment effect, and China's mangrove has 12 sections 15 to belong to 27 kinds, is widely distributed in China southeastern coast coastline.According to medicinal textual criticism to mangrove among the people; China's history with long-term medical mangrove plant among the people; Like the specific drug of positive Rhizophora apiculata Blume for treatment renal tuberculosis, lithangiuria etc., the red eggplant winter is used to treat red water, and Bruguiera gymnoihiza (L.) Savigny. is really treated diabetes; The LAOSHULE root has leukemia and anti-hepatitis B is active, and the Bruguiera sexangula (Lour) Poir bark extract has the sarcoma S180 of inhibition and Lewis lung cancer is active.Record 3 kinds of mangroves (LAOSHULE, extra large Fructus Mangifera Indicae and Cortex seu flos hibisci tiliacei) and medicinal efficacy thereof in " national Chinese herbal medicine compilation " (1978).According to statistics, the nearly half the mangrove of China has therapeutic use to multiple disease.Yet, the active component and the Study on mechanism thereof of Rhizophora apiculata Blume medicinal plants are rarely reported at home.And in the world, particularly country in Southeast Asia delivers chemical constituent and bioactive paper with mangrove at international magazine in recent years in succession, shows that in the world chemical constituent multiformity and the biological activity thereof to mangrove attracts great attention.
People (CN101077345A) such as the human diseases cara gene Lin Wenhan of Peking University find that the new diterpene compound Tagalsin C and the homologue thereof that contain in the mangrove have anti-tumor activity.But about the report that from mangrove, extracts Tagalsin C seldom, especially do not adopt biological enzyme to extract the bibliographical information of Tagalsin C.Therefore, the inventor has made the present invention finally through big quantity research.
[summary of the invention]
[technical problem that will solve]
The purpose of this invention is to provide a kind of Rhizophora apiculata Blume extracting solution.
Another object of the present invention provides a kind of method for preparing of said Rhizophora apiculata Blume extracting solution.
[technical scheme]
The objective of the invention is to provides a kind of mangrove extracting solution that contains new diterpene-kind compound Tagalsin C and preparation method thereof to the problems referred to above, makes the extracting solution that makes have the broad-spectrum selectivity and kills tumor promotion.
The present invention adopts following technical proposals to realize.
The present invention relates to a kind of Rhizophora apiculata Blume extracting solution, it is characterized in that it contains the C in the new diterpene-kind compound Tagalsin of said extracting solution weight 0.001-0.25 weight %.
The invention still further relates to the method for preparing of said Rhizophora apiculata Blume extracting solution, it is characterized in that the step of this method is following:
A, pulverizing
The extra dry red wine tree plant is crushed to the 20-200 order, joins the mangrove powder that obtains and extract in the still;
B, antibacterial
According to described mangrove powder: the weight ratio 1 of water: 3-20 is toward steps A) add water in the mangrove powder that obtains and obtain a kind of slurry; Under agitation the mangrove powder slurry that obtains is heated to 75-85 ℃, under this temperature, sterilized 8-12 minute with heating rate 5-15 ℃/minute;
C, cooling
With step B) the sterilization mangrove powder slurry that obtains is cooled to 40-60 ℃;
E, enzymolysis
Toward step C) add in said mangrove weight 0.01-0.5% pectase and 0.2-0.4% cellulase in the cooling mangrove powder slurry that obtains,, hydrolysis temperature carried out enzymolysis 60-300 minute under being 40-60 ℃ and enzymolysis pH4-5 condition;
F, enzyme denaturing
In step e) the mangrove powder slurry of enzymolysis heated under temperature 75-85 ℃ enzyme denaturing 8-12 minute, cooled off behind the enzyme denaturing and centrifugal filtration, obtained supernatant 1 and raffinate;
G, ultrasonic extraction
Toward step F) add 95% alcoholic solution in the mangrove raffinate that obtains; The volume ratio of its mangrove raffinate and alcoholic solution is 1: 5-15; Under 55-78 ℃ of constant temperature and frequency 18KHz, carrying out auxiliary ultrasonic extracted 3.5-4 hour; Cool off then and carry out centrifugal filtration, obtain supernatant 2;
H concentrates
Supernatant 1 and supernatant 2 are merged, under the 100-800Pa vacuum decompression, concentrate, be concentrated into when soluble solid content reaches 45-60% in the supernatant and stop to concentrate, products obtained therefrom is the mangrove extracting solution.
In the present invention, described mangrove is selected from one or more in this plant roots, stem, leaf, branch, flower or the fruit.
According to a kind of preferred implementation, described centrifugal filtration can be adopted the cloth bag filtration or adopt the filter pressing method to carry out.
According to another kind of preferred implementation, described concentrating can be that normal pressure concentrates.
Below the present invention will be described in more detail.
The present invention relates to a kind of Rhizophora apiculata Blume extracting solution, it contains the C in the new diterpene-kind compound Tagalsin of said extracting solution weight 0.001-0.25 weight %.
CN101077345A discloses Tagalsin C and homologue Tagalsins A thereof, B, D, E, F, the application of G in the preparation antitumor drug.This series compound has membrane permeability and broad-spectrum kills tumor promotion; Can kill and wound people early children's grain acute leukemia cells HL-60, human myeloma cell IM9 etc.; And normal cell people kidney blastocyte 293 is not had tangible kill capability with people liver diploid cell L02, can be applicable to prepare the medicine of treating tumor etc.
The invention still further relates to the method for preparing of said Rhizophora apiculata Blume extracting solution.The step of this Rhizophora apiculata Blume extracting solution method for preparing is following:
At first, mangrove raw material pulverizing.Use normally used disintegrating apparatus in processing technique of Chinese herbs is crushed to the 20-200 order with the extra dry red wine tree plant, preferably 40-150 order, more preferably 60-120 order.Described disintegrating apparatus is the normally used disintegrating apparatus of people in the art, also is the Chinese crude drug disintegrating apparatus of mass selling in the market.In the present invention, described mangrove is selected from one or more in this plant roots, stem, leaf, branch, flower or the fruit.
The mangrove powder that obtains after the pulverizing installs to and extracts in the still.In the present invention; Described extraction still should be appreciated that it is a kind of reaction vessel from mangrove powder effective component extracting, and this reaction vessel for example can be that rustless steel tank reactor, autoclave pressure reaction vessel or any other can be implemented the reaction vessel of effective component extracting from plant.
Then, mangrove powder antibacterial.According to described mangrove powder: the weight ratio 1 of water: 3-20 adds water in said mangrove powder; Stirring obtains mangrove powder slurry; This slurry under agitation is heated to 75-85 ℃ with heating rate 5-15 ℃/minute with the mangrove powder slurry that obtains, and under this temperature, sterilizes 8-12 minute.Preferably, heating rate is controlled at 8-12 ℃/minute, and mangrove powder slurry temperature is controlled at 78-82 ℃, in this temperature range, sterilizes 9-10 minute.According to using type of reactor, can select direct heating mode or indirect mode.The direct heating mode is with steam direct heating mangrove powder slurry, and the indirect mode is to flow through reactor jacket heating mangrove powder slurry through adding hot fluid, and these mode of heatings all are that the technical staff in present technique field knows.The total plate count method that mangrove powder slurry sterilization situation can adopt the present technique field to adopt usually checks, when mangrove powder slurry total plate count can think qualified during less than 20/milliliter, otherwise need sterilize again.
Then, cool off after the sterilization of mangrove powder slurry.Usually, place air to naturally cool to 40-60 ℃ the above-mentioned sterilization mangrove powder slurry that obtains; Can certainly adopt other cooling means to cool off, for example cool off toward the logical tap water of reactor jacket.
Then, cooling mangrove powder slurry carries out enzymolysis.In cooling mangrove powder slurry, add, under hydrolysis temperature is 40-60 ℃ and enzymolysis pH4-5 condition, carried out enzymolysis 60-300 minute in said mangrove weight 0.01-0.5% pectase and 0.2-0.4% cellulase.Preferably, in cooling mangrove powder slurry, add in said mangrove weight 0.1-0.4% pectase and 0.2-0.3% cellulase.
Cellulase can make the mangrove cell wall breaking cellular wall of compact structure; Therefore help the intracellular effective ingredient stripping of Rhizophora apiculata Blume; Pectase can be hydrolyzed insoluble matters such as the starch in the mangrove, protein, becomes DDGS by insoluble matter, thereby improves enzymolysis efficiency.The cellulase that uses is the cellulase product that Wuxi company of outstanding ability section produces with the grand mcroorganism Engineering Co., Ltd of the trade name outstanding ability P200 of section product sold or Shandong.The pectase that uses is the pectase that Novozymes Company sells with trade name AFP XXL.
Enzymolysis mangrove powder slurry carries out enzyme denaturing.The mangrove powder slurry of enzymolysis was heated under temperature 75-85 ℃ enzyme denaturing 8-12 minute, and the mangrove powder slurry behind the enzyme denaturing cools off, and carries out centrifugal filtration again, can obtain supernatant 1 and raffinate like this.Carrying out the type of cooling behind the mangrove powder slurry enzyme denaturing can be identical with the type of cooling after the sterilization of mangrove powder slurry.Centrifugal filtration generally is to use filter centrifugal under 8000 rev/mins of centrifugation rates, carrying out centrifugalize 10-20 minute, obtains supernatant 1 and raffinate, and described filter centrifugal for example is a U.S. BECKMAN centrifuge.
Follow the ultrasonic extraction of raffinate.In the mangrove raffinate that obtains, add 95% alcoholic solution; The volume ratio of its mangrove raffinate and alcoholic solution is 1: 5-15; Under 55-78 ℃ of constant temperature and frequency 18KHz, carry out auxiliary ultrasonic and extracted 3.5-4 hour, cool off then and carry out centrifugal filtration, obtain supernatant 2.The employed equipment of ultrasonic extraction is normally used in the art equipment, for example the ultrasonic equipment of Hangzhou Success Ultrasonic Equipment Co., Ltd's production.Cool off the mode and the equipment and described above identical that adopt with centrifugal filtration.In the present invention, described centrifugal filtration can be adopted the cloth bag filtration or adopt the filter pressing method to carry out.
Then supernatant 1 is merged with supernatant 2 and concentrate.Supernatant 1 and supernatant 2 are merged, under the 100-800Pa vacuum decompression, concentrate, be concentrated into when soluble solid content reaches 45-60% in the supernatant and stop to concentrate, products obtained therefrom is the mangrove extracting solution.In the present invention; The employed equipment of said merging supernatant concentration is normally used in the art equipment, for example Wuxi City avenge unrestrained fermentation engineering instrument factory with the dynamic hot reflux extracting-concentration machine product sold of trade name or Shanghai legendary god of farming machinery company limited with trade name falling film evaporator product sold.In the present invention, described concentrating also can be that normal pressure concentrates.
Can adopt gas chromatogram (GC) analytical method to be determined at the new diterpene-kind compound Tagalsin C content in the products obtained therefrom mangrove extracting solution.
[beneficial effect]
It is raw material that the present invention selects mangrove for use, extracts effective ingredient noval chemical compound TagalsinC wherein.This method for distilling efficient is high, simple and efficient to handle, and cost is low, has wide application prospect.
[specific embodiment]
Embodiment 1:
The leaf (moisture is 10%) that takes by weighing 100 kilograms mangrove uses the MZ200 type Chinese medicine grinder of Qingdao Mai Kelong powder technology equipment company limited production to be crushed to 30 orders; The leaf of the mangrove of pulverizing is added in the extraction still, add 500 kg of water.Under condition of stirring, the extraction still that mangrove is housed is carried out pasteurization, sterilization temperature is 80 ℃, keeps 10 minutes.After the antibacterial, carry out natural cooling to extracting still.When temperature drops to 60 ℃, stop cooling.Keep system temperature at 60 ℃, add by 0.01% of mangrove weight (dry weight) that pectase that Novozymes Company sells with trade name AFP XXL and 0.4% adding Wuxi are outstanding can company of section carry out enzymolysis with the outstanding cellulase that can the P200 of section sale of trade name.The time of enzymolysis is 60 minutes, and the pH of enzymolysis is controlled at 5.Enzymolysis heats enzyme denaturing after accomplishing, and the temperature of enzyme denaturing is 80 ℃, and the time of enzyme denaturing is 10 minutes.The enzyme denaturing postcooling is to room temperature, and adopts centrifugal the filtration, 490 kilograms of supernatant 1.Filtration obtains 110 kilograms of residues, adds 550 kilograms of 95% alcoholic solution toward this residue, and the ultrasonic equipment that uses Hangzhou Success Ultrasonic Equipment Co., Ltd to produce extracted 4 hours in 55 ℃ of constant temperature auxiliary ultrasonic of temperature, and ultrasound condition is frequency 18KHz.Extract and accomplish postcooling and carry out centrifugal filtration, get 580 kilograms of supernatant 2.
Supernatant 1 and supernatant 2 are merged; Under the 500Pa vacuum decompression, concentrate; Be concentrated into that soluble solid content reaches at 45% o'clock in the supernatant; Stop to concentrate, products obtained therefrom is the mangrove extracting solution that contains new diterpene-kind compound Tagalsin C, adopts gas chromatogram (GC) analytical method to confirm that this mangrove extracting solution contains 0.046% new diterpene-kind compound Tagalsin C.
Embodiment 2:
The leaf (moisture is 10%) that takes by weighing 100 kilograms mangrove uses the MZ200 type Chinese medicine grinder of Qingdao Mai Kelong powder technology equipment company limited production to be crushed to 30 orders; The leaf of the mangrove of pulverizing is added in the extraction still, add 1800 kg of water.Under condition of stirring, the extraction still that mangrove is housed is carried out pasteurization, sterilization temperature is 80 ℃, keeps 10 minutes.After the antibacterial, cool off toward extracting the logical tap water of still chuck.When temperature drops to 40 ℃, stop cooling.Keep system temperature at 40 ℃, add by 0.5% of mangrove weight (dry weight) that pectase that Novozymes Company sells with trade name AFP XXL and 0.2% adding Wuxi are outstanding can company of section carry out enzymolysis with the outstanding cellulase that can the P200 of section sale of trade name.The time of enzymolysis is 300 minutes, and the pH of enzymolysis is controlled at 5.Enzymolysis heats enzyme denaturing after accomplishing, and the temperature of enzyme denaturing is 80 ℃, and the time of enzyme denaturing is 10 minutes.The enzyme denaturing postcooling is to room temperature, and adopts centrifugal the filtration, 1775 kilograms of supernatant 1.Filtration obtains 115 kilograms of residues, adds 1725 kilograms of 95% alcoholic solution toward this residue, and the ultrasonic equipment that uses Hangzhou Success Ultrasonic Equipment Co., Ltd to produce extracted 3.5 hours in 55 ℃ of constant temperature auxiliary ultrasonic of temperature, and ultrasound condition is frequency 18KHz.Extract and accomplish postcooling and carry out centrifugal filtration, get 1740 kilograms of supernatant 2.
Supernatant 1 and supernatant 2 are merged, under the 400Pa vacuum decompression, concentrate, be concentrated into that soluble solid content reaches at 60% o'clock in the supernatant, stop to concentrate, products obtained therefrom is the mangrove extracting solution that contains new diterpene-kind compound Tagalsin C.Adopt gas chromatogram (GC) analytical method to confirm that this mangrove extracting solution contains 0.052% new diterpene-kind compound Tagalsin C.
Claims (5)
1. the method for preparing of a Rhizophora apiculata Blume extracting solution is characterized in that the step of this method is following:
A, pulverizing
The extra dry red wine tree plant is crushed to the 20-200 order, joins the mangrove powder that obtains and extract in the still;
B, antibacterial
According to described mangrove powder: the weight ratio 1 of water: 3-20 is toward steps A) add water in the mangrove powder that obtains and obtain a kind of slurry; Under agitation the mangrove powder slurry that obtains is heated to 75-85 ℃, under this temperature, sterilized 8-12 minute with heating rate 5-15 ℃/minute;
C, cooling
With step B) the sterilization mangrove powder slurry that obtains is cooled to 40-60 ℃;
E, enzymolysis
Toward step C) add in said mangrove weight 0.01-0.5% pectase and 0.2-0.4% cellulase in the cooling mangrove powder slurry that obtains,, hydrolysis temperature carried out enzymolysis 60-300 minute under being 40-60 ℃ and enzymolysis pH4-5 condition;
F, enzyme denaturing
In step e) the mangrove powder slurry of enzymolysis heated under temperature 75-85 ℃ enzyme denaturing 8-12 minute, cooled off behind the enzyme denaturing and centrifugal filtration, obtained supernatant 1 and raffinate;
G, ultrasonic extraction
Toward step F) add 95% alcoholic solution in the mangrove raffinate that obtains; The volume ratio of its mangrove raffinate and alcoholic solution is 1: 5-15; Under 55-78 ℃ of constant temperature and frequency 18KHz, carrying out auxiliary ultrasonic extracted 3.5-4 hour; Cool off then and carry out centrifugal filtration, obtain supernatant 2;
H concentrates
Supernatant 1 and supernatant 2 are merged; Under the 100-800Pa vacuum decompression, concentrate; Be concentrated into when soluble solid content reaches 45-60% in the supernatant and stop to concentrate; Products obtained therefrom is the mangrove extracting solution, and said mangrove extracting solution contains the C in the new diterpene-kind compound Tagalsin of said extracting solution weight 0.001-0.25 weight %.
2. method for preparing according to claim 1 is characterized in that described mangrove is selected from one or more in this plant roots, stem, leaf, branch, flower or the fruit.
3. method for preparing according to claim 1 is characterized in that in cooling mangrove powder slurry, adding in said mangrove weight 0.1-0.4% pectase and 0.2-0.3% cellulase.
4. method for preparing according to claim 1 is characterized in that described centrifugal filtration employing cloth bag filtration or adopts the filter pressing method to carry out.
5. method for preparing according to claim 1 is characterized in that in said concentrated H step, concentrates alternative vacuum decompression with normal pressure and concentrates.
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| CN103373912B (en) * | 2012-04-25 | 2017-07-14 | 北京大学 | The method that antitumor lead compound Tagalsin C are prepared using Tagalsin E and Tagalsin G |
| CN102783627A (en) * | 2012-08-08 | 2012-11-21 | 天宁香料（江苏）有限公司 | Preparation method for blending-type tamarind fruit essence and tamarind fruit essence therefrom |
| CN102754784B (en) * | 2012-08-08 | 2013-06-19 | 天宁香料（江苏）有限公司 | Method for preparing tamarind fruit extract and application of same in edible essence |
| CN113621297A (en) * | 2021-08-17 | 2021-11-09 | 深圳先进技术研究院 | Eco-friendly antibacterial coating material and preparation method and application thereof |
| KR102648506B1 (en) * | 2021-11-08 | 2024-03-18 | (주)코이즈 | Cosmetic composition containing mangrove root and guaajava leaf |
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| CN101077345A (en) * | 2006-05-23 | 2007-11-28 | 北京大学 | Application of Tagalsin C and its homologous compound in preparing anti-tumor medicine |
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| CN101077345A (en) * | 2006-05-23 | 2007-11-28 | 北京大学 | Application of Tagalsin C and its homologous compound in preparing anti-tumor medicine |
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