CN103690572A - Preparation method of inonotus obliquus tea powder - Google Patents

Preparation method of inonotus obliquus tea powder Download PDF

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CN103690572A
CN103690572A CN201310712138.XA CN201310712138A CN103690572A CN 103690572 A CN103690572 A CN 103690572A CN 201310712138 A CN201310712138 A CN 201310712138A CN 103690572 A CN103690572 A CN 103690572A
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inonqqus obliquus
tea powder
preparation
extracting solution
solution
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CN103690572B (en
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刘俊梅
杨庆贺
李琢伟
王丹
王璐
王辉
王庆
杨盼盼
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Mesui Jilin Technology Co ltd
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Abstract

The invention discloses a preparation method of inonotus obliquus tea powder. The preparation method comprises the following steps: extracting inonotus obliquus used as a raw material so as to obtain a polysaccharide extraction solution and a triterpenoid extraction solution; mixing the polysaccharide extraction solution and the triterpenoid extraction solution at a ratio of 1: 1 to obtain a mixed extraction solution; sequentially performing rotary evaporation and concentration and centrifugal treatment on the mixed extraction solution and taking a supernatant liquid; mixing the supernatant liquid with maltodextrin to obtain a uniform solution, and performing spray-drying treatment to prepare the inonotus obliquus tea powder. The inonotus obliquus tea powder has the advantages of simple preparation process, low preparation cost, relatively high content of active substances, effects of enabling organoleptic states to be easily accepted and enabling active ingredients to be easily digested and absorbed by human bodies, rapid onset of action, long-acting property, and relatively strong popularization and application value.

Description

A kind of preparation method of Inonqqus obliquus tea powder
Technical field
The invention belongs to Inonqqus obliquus tea powder preparing technical field, relate in particular to a kind of preparation method of Inonqqus obliquus tea powder.
Background technology
Inonqqus obliquus, is again Phaeoporus obliquus, the brown pore fungi of birch cancer, the fine pore fungi of inclined tube, Polyporus badius.Be born in the dried-up upper of trees under the bark of standing tree or after felling of living such as Betula platyphylla Suk., silvery birch, elm, Folium Et Cacumen Alni Japonicae, its sclerotium can be after felling dried-up on existence for 6 years.Mainly be distributed at home Heilongjiang Province, Changbaishan area, Jilin Province, etc. area.Its composition mainly contains lanosterol type triterpenes, Inonqqus obliquus alcohol and inonotus obliquus, melanin class, folic acid derivatives, and aromatic substance, lignin, the acid of bolt bacterium, the chemical compositions such as tannin, what wherein play main pharmacological is lanosterol type triterpenes, Inonqqus obliquus alcohol, inonotus obliquus and lignin. there is opposing hepatocarcinoma, gastric cancer, pulmonary carcinoma, cervical cancer, breast carcinoma, skin carcinoma, rectal cancer, the kinds of tumor cells such as lymph, and AIDS virus resisting, infection, treatment diabetes, blood pressure lowering regulates blood fat, anti-body aging, the pharmacological actions such as enhancing immunity.
Summary of the invention
The invention provides a kind of preparation method of Inonqqus obliquus tea powder, be intended to solve the technique of extracting polysaccharose substance and triterpene substance at present from Inonqqus obliquus, process is complicated, extraction efficiency is low, the preparation method of existing Inonqqus obliquus tea powder of while, complex process, active substance content is lower, sense organ state is difficult for being accepted, the problem that active ingredient is not easily digested.
The object of the present invention is to provide a kind of preparation method of Inonqqus obliquus tea powder, the preparation method of this Inonqqus obliquus tea powder comprises the following steps:
Step 1, take Inonqqus obliquus as raw material, extracts and obtains polysaccharide extracting solution and triterpenes extracting solution;
Step 2, mixes with triterpenes extracting solution polysaccharide extracting solution with 1: 1 ratio, obtain mixed extract;
Step 3, is rotated evaporation and concentration and centrifugal treating successively to mixed extract, gets supernatant;
Step 4, is mixed into homogeneous solution by supernatant and maltodextrin, and Inonqqus obliquus tea powder is made in spray-dried processing.
Further, in step 1, take Inonqqus obliquus as raw material, the implementation method of extracting acquisition polysaccharide extracting solution and triterpenes extracting solution is:
Selected Inonqqus obliquus is carried out to manual break process;
The Inonqqus obliquus of manual break process is carried out to water soaking processing, adopt heating decocting in water supersound extraction again, filter and obtain polysaccharide extracting solution;
Filtering residue is carried out to soak with ethanol processing, adopt water-bath supersound extraction again, filter and obtain triterpenes extracting solution.
Further, when the Inonqqus obliquus of manual break process is carried out to water soaking processing, the condition of water soaking is: ratio is 1: 10 (w/v), soak at room temperature 24 hours; The condition of soak with ethanol is: ratio is 1: 10 (w/v), soak at room temperature 24 hours, and concentration of alcohol is 90%.
Further, in step 3, after mixed extract rotary evaporation is concentrated, concentrated 4.2 times of volume, concentration is 2.3 Baume degrees.
Further, in step 3, after mixed extract rotary evaporation is concentrated, the condition of centrifugal treating is: centrifugal speed 7500r/min, centrifugation time 10min.
Further, in step 4, when supernatant and maltodextrin are mixed into homogeneous solution, the addition of maltodextrin is 10% of solution.
Further, in step 4, the homogeneous solution that supernatant and maltodextrin are mixed into carries out spray-dired condition and is: inlet temperature is 120 ℃, and leaving air temp is 60 ℃, and flow velocity is: 1.0ml/min.
The preparation method of Inonqqus obliquus tea powder provided by the invention, take Inonqqus obliquus as raw material, extracts and obtains polysaccharide extracting solution and triterpenes extracting solution; Polysaccharide extracting solution is mixed with 1: 1 ratio with triterpenes extracting solution, obtain mixed extract; Mixed extract is rotated to evaporation and concentration and centrifugal treating successively, gets supernatant; Supernatant and maltodextrin are mixed into homogeneous solution, and spray-dried processing, makes Inonqqus obliquus tea powder; This Inonqqus obliquus tea powder, preparation technology is simple, and preparation cost is low, and active substance content is higher, and sense organ state is easily accepted, and active ingredient is easily digested, instant effect, drug effect is long, has stronger propagation and employment and is worth.
Accompanying drawing explanation
Fig. 1 is the realization flow figure of the preparation method of the Inonqqus obliquus tea powder that provides of the embodiment of the present invention;
Fig. 2 is provide Inonqqus obliquus is manually diced and after micronizing processes of the embodiment of the present invention, the comparison schematic diagram of active substance component content in Inonqqus obliquus;
Fig. 3 is that the C18 chromatographic column that in the soak with ethanol that provides of the embodiment of the present invention, four kinds of schemes are extracted active substance content in Inonqqus obliquus detects comparison diagram, in figure, represent first water-bath supersound process again for No. 1, represent supersound process No. 2, represent water-bath No. 3, untreated after representing for No. 4 to soak;
Fig. 4 is that the nh 2 column chromatographic column that in the soak with ethanol that provides of the embodiment of the present invention, four kinds of schemes are extracted active substance content in Inonqqus obliquus detects comparison diagram, in figure, represent first decocting in water supersound process again for No. 1, represent supersound process No. 2, represent decocting in water No. 3, untreated after representing for No. 4 to soak;
Fig. 5 is that the C18 chromatographic column that in the water soaking that provides of the embodiment of the present invention, four kinds of schemes are extracted active substance content in Inonqqus obliquus detects comparison diagram, in figure, represent first decocting in water supersound process again for No. 1, represent supersound process No. 2, represent decocting in water processing for No. 3, untreated after representing for No. 4 to soak;
Fig. 6 is that the nh 2 column chromatographic column that in the water soaking that provides of the embodiment of the present invention, four kinds of schemes are extracted active substance content in Inonqqus obliquus detects comparison diagram, represents first decocting in water supersound process again in figure for No. 1; Represent supersound process No. 2; Represent decocting in water No. 3; Untreated after representing for No. 4 to soak.
The specific embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is described in further detail.Should be appreciated that specific embodiment described herein is only in order to explain the present invention, and be not used in restriction invention.
Fig. 1 shows the realization flow of the preparation method of the Inonqqus obliquus tea powder that the embodiment of the present invention provides.
The preparation method of this Inonqqus obliquus tea powder comprises the following steps:
Step S101, take Inonqqus obliquus as raw material, extracts and obtains polysaccharide extracting solution and triterpenes extracting solution;
Step S102, mixes with triterpenes extracting solution polysaccharide extracting solution with 1: 1 ratio, obtain mixed extract;
Step S103, is rotated evaporation and concentration and centrifugal treating successively to mixed extract, gets supernatant;
Step S104, is mixed into homogeneous solution by supernatant and maltodextrin, and Inonqqus obliquus tea powder is made in spray-dried processing.
In embodiments of the present invention, in step S101, take Inonqqus obliquus as raw material, the implementation method of extracting acquisition polysaccharide extracting solution and triterpenes extracting solution is:
Selected Inonqqus obliquus is carried out to manual break process;
The Inonqqus obliquus of manual break process is carried out to water soaking processing, adopt heating decocting in water supersound extraction again, filter and obtain polysaccharide extracting solution;
Filtering residue is carried out to soak with ethanol processing, adopt water-bath supersound extraction again, filter and obtain triterpenes extracting solution.
In embodiments of the present invention, when the Inonqqus obliquus of manual break process is carried out to water soaking processing, the condition of water soaking is: ratio is 1: 10 (w/v), soak at room temperature 24 hours; The condition of soak with ethanol is: ratio is 1: 10 (w/v), soak at room temperature 24 hours, and concentration of alcohol is 90%.
In embodiments of the present invention, in step S103, after mixed extract rotary evaporation is concentrated, concentrated 4.2 times of volume, concentration is 2.3 Baume degrees.
In embodiments of the present invention, in step S103, after mixed extract rotary evaporation is concentrated, the condition of centrifugal treating is: centrifugal speed 7500r/min, centrifugation time 10min.
In embodiments of the present invention, in step S104, when supernatant and maltodextrin are mixed into homogeneous solution, the addition of maltodextrin is 10% of solution.
In embodiments of the present invention, in step S104, the homogeneous solution that supernatant and maltodextrin are mixed into carries out spray-dired condition and is: inlet temperature is 120 ℃, and leaving air temp is 60 ℃, and flow velocity is: 1.0ml/min.
Below in conjunction with drawings and the specific embodiments, application principle of the present invention is further described.
The invention provides active substance extracting method in Inonqqus obliquus, selected Inonqqus obliquus raw material is through break process, first with certain solid-liquid ratio, carry out water soaking, with four kinds of extracting method, process and extract wherein polysaccharide composition respectively afterwards, it is polysaccharide material extracting solution that filtration treatment obtains filtrate, filtering residue is used soak with ethanol again, with four kinds of extracting method, process and extract wherein triterpenes composition respectively afterwards, obtaining after filtration filtrate is triterpenes class material extracting solution, by high-efficient liquid phase chromatogram technology, the effective ingredient in extracting solution is carried out to qualitative and quantitative analysis.
During Inonqqus obliquus raw material process break process, adopt the little manual break process of loss of effective components degree;
Inonqqus obliquus raw material first passes through water soaking, after extracting, passes through soak with ethanol again, and the condition of water soaking is: ratio is 1: 10 (w/v), soak at room temperature, 24 hours; The condition of soak with ethanol: ratio is 1: 10 (w/v), soak at room temperature, 24 hours, concentration of alcohol was 90%;
The extraction process of effective ingredient adopts the decocting in water ultrasonic and soaked bath of alcohol leaching ultrasonic technique more again;
Application high performance liquid chromatography detects effective ingredient.
The invention provides a kind of preparation method of Inonqqus obliquus tea powder, by polysaccharide extracting solution and triterpenes extracting solution to be mixed to get mixed extract at 1: 1, mixed extract is through rotary evaporation, after centrifugal treating, get supernatant, and be mixed into homogeneous solution with maltodextrin, maltodextrin is as filler, and solution is through the dry Inonqqus obliquus tea powder of making of spraying.
Above-mentioned polysaccharide extracting solution and triterpenes extracting solution are mixed as raw material, after mixed extract is concentrated, concentrated 4.2 times of volume, concentration is 2.3 Baume degrees.
Concentrated solution is through centrifugal treating, and centrifugal condition is 7500r/min, and 10min, obtains supernatant.
Supernatant and maltodextrin are mixed into homogeneous solution with certain proportion, and the addition of maltodextrin is 10% of solution.
Solution is through the dry Inonqqus obliquus tea powder that obtains of spraying, and spraying drying condition is: inlet temperature is 120 ℃, and leaving air temp is 60 ℃, and flow velocity is: 1.0ml/min.
Inonqqus obliquus pre-treatment is as follows:
Inonqqus obliquus break process is carried out manual handle and two kinds of method comparisons of mechanical treatment, and detects and select a kind of extracting method that component content is higher that extracts according to high performance liquid chromatography; For difference, be extracted into afterwards and respectively that sorting is soaked in water and alcohol soaks.The condition of water soaking is: ratio is 1: 10 (w/v), soak at room temperature, 24 hours; The condition of soak with ethanol: ratio is 1: 10 (w/v), soak at room temperature, 24 hours, concentration of alcohol was 90%.
Extracts active ingredients scheme in Inonqqus obliquus:
Scheme 1: directly detect after immersion;
Scheme 2: after soaking, feed liquid is carried out decocting in water (alcohol: water-bath) extract, extraction conditions is 90 ℃, 30min;
Scheme 3: after soaking, feed liquid is carried out supersound extraction, and extraction conditions is 60 ℃, 30min;
Scheme 4: after soaking, feed liquid is first carried out decocting in water (alcohol: water-bath) heat, heating condition is 90 ℃, 30min; Carry out supersound extraction, extraction conditions is 60 ℃, 30min again.
Extracting solution detects through high performance liquid chromatogram, detects respectively by the chromatographic column of nh 2 column and two kinds of models of C18, and wherein nh 2 column is mainly for polysaccharide material in Inonqqus obliquus, and C18 detects mainly for triterpene substance in Inonqqus obliquus.
Select the most effective extracting method to carry out active substance extracting method, extract respectively polysaccharide and triterpene substance, evenly mix, and then be rotated 4.2 times of concentrated solutions of evaporation and concentration.
In the preparation method of Inonqqus obliquus tea powder, after concentrated solution is centrifugal, gets supernatant and add the dry powder of making of 10% maltodextrin spraying.
Test specimen:
Primary raw material: Inonqqus obliquus, food stage ethanol, distilled water, chromatographic grade acetonitrile, hplc grade methanol;
Testing equipment: supersound extraction instrument, high performance liquid chromatograph, C18 chromatographic column, nh 2 column, Rotary Evaporators, electromagnetic oven, spray dryer.
2 can find out with reference to the accompanying drawings, and raw material detects effective ingredient wherein peak height through manually dicing will illustrate that micronizing is very large for loss of effective components in Inonqqus obliquus far above micronizing, and therefore manually dicing is first-selected processing method.
3 can find out with reference to the accompanying drawings, soak with ethanol Inonqqus obliquus, after four kinds of extracting method are processed, through C18 chromatographic column, detect, find that extracted amount is descending as follows successively: first water-bath again supersound process > supersound process > water bath processing > is untreated after soaking.And C18 chromatographic column can detect the material under ultraviolet light with certain absworption peak.Illustrate in detected absworption peak it may is the triterpene substance extracting.According to appearance time, 6.5 is identical with the appearance time of solvent peak with about 12.5min, can judge that this is impurity, can judge 20,27,31.5 and 41.5min about go out peak material may be the active substance extracting from Inonqqus obliquus.
4 can find out with reference to the accompanying drawings, and alcohol soaks Inonqqus obliquus, through nh 2 column chromatographic column, detect and do not have peak to occur, that is to say that alcohol extraction is not by polysaccharide extracts active ingredients wherein out.
5 can find out with reference to the accompanying drawings, and water soaking Inonqqus obliquus detects and do not have peak to occur through C18 chromatographic column, because there is no absworption peak under ultraviolet light, that is to say that water extraction is not by triterpenes extracts active ingredients wherein out.
6 can find out with reference to the accompanying drawings, through nh 2 column, detect, in 10min left and right, there is peak to occur, illustrate after water extraction and have carbohydrate content in solution, and find that extracted amount is descending as follows successively: first decocting in water again supersound process > supersound process > decocting in water is untreated after processing > and soaking.
As can be seen here, alcohol extraction can extract triterpene substance in Inonqqus obliquus, and water extraction can extract polysaccharide composition in Inonqqus obliquus, and Inonqqus obliquus is ultrasonic best with alcohol extraction water-bath extraction effect again through decocting in water after soaking.
The preparation method of the Inonqqus obliquus tea powder that the embodiment of the present invention provides, take Inonqqus obliquus as raw material, extracts and obtains polysaccharide extracting solution and triterpenes extracting solution; Polysaccharide extracting solution is mixed with 1: 1 ratio with triterpenes extracting solution, obtain mixed extract; Mixed extract is rotated to evaporation and concentration and centrifugal treating successively, gets supernatant; Supernatant and maltodextrin are mixed into homogeneous solution, and spray-dried processing, makes Inonqqus obliquus tea powder; This Inonqqus obliquus tea powder, preparation technology is simple, and preparation cost is low, and active substance content is higher, and sense organ state is easily accepted, and active ingredient is easily digested, instant effect, drug effect is long, has stronger propagation and employment and is worth.
These are only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.

Claims (7)

1. a preparation method for Inonqqus obliquus tea powder, is characterized in that, the preparation method of this Inonqqus obliquus tea powder comprises the following steps:
Step 1, take Inonqqus obliquus as raw material, extracts and obtains polysaccharide extracting solution and triterpenes extracting solution;
Step 2, mixes with triterpenes extracting solution polysaccharide extracting solution with 1: 1 ratio, obtain mixed extract;
Step 3, is rotated evaporation and concentration and centrifugal treating successively to mixed extract, gets supernatant;
Step 4, is mixed into homogeneous solution by supernatant and maltodextrin, and Inonqqus obliquus tea powder is made in spray-dried processing.
2. the preparation method of Inonqqus obliquus tea powder as claimed in claim 1, is characterized in that, in step 1, take Inonqqus obliquus as raw material, and the implementation method of extracting acquisition polysaccharide extracting solution and triterpenes extracting solution is:
Selected Inonqqus obliquus is carried out to manual break process;
The Inonqqus obliquus of manual break process is carried out to water soaking processing, adopt heating decocting in water supersound extraction again, filter and obtain polysaccharide extracting solution;
Filtering residue is carried out to soak with ethanol processing, adopt water-bath supersound extraction again, filter and obtain triterpenes extracting solution.
3. the preparation method of Inonqqus obliquus tea powder as claimed in claim 2, is characterized in that, when the Inonqqus obliquus of manual break process is carried out to water soaking processing, the condition of water soaking is: ratio is 1: 10 (w/v), soak at room temperature 24 hours; The condition of soak with ethanol is: ratio is 1: 10 (w/v), soak at room temperature 24 hours, and concentration of alcohol is 90%.
4. the preparation method of Inonqqus obliquus tea powder as claimed in claim 1, is characterized in that, in step 3, and after mixed extract rotary evaporation is concentrated, concentrated 4.2 times of volume, concentration is 2.3 Baume degrees.
5. the preparation method of Inonqqus obliquus tea powder as claimed in claim 1, is characterized in that, in step 3, after mixed extract rotary evaporation is concentrated, the condition of centrifugal treating is: centrifugal speed 7500r/min, centrifugation time 10min.
6. the preparation method of Inonqqus obliquus tea powder as claimed in claim 1, is characterized in that, in step 4, when supernatant and maltodextrin are mixed into homogeneous solution, the addition of maltodextrin is 10% of solution.
7. the preparation method of Inonqqus obliquus tea powder as claimed in claim 1, it is characterized in that, in step 4, the homogeneous solution that supernatant and maltodextrin are mixed into carries out spray-dired condition and is: inlet temperature is 120 ℃, leaving air temp is 60 ℃, and flow velocity is: 1.0ml/min.
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CN116120480A (en) * 2023-01-06 2023-05-16 湖南杰萃生物技术有限公司 Method for simultaneously extracting inonotus obliquus polysaccharide and inonotus obliquus element

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Publication number Priority date Publication date Assignee Title
CN104004106A (en) * 2014-04-28 2014-08-27 杨庆贺 Method for extracting effective substances in inonotus obliquus and preparation method for teabag
CN105410240A (en) * 2015-12-04 2016-03-23 潘玉来 Inonotus obliquus health tea and production method thereof
CN105558056A (en) * 2015-12-30 2016-05-11 天津横天生物科技有限公司 Inonotus obliquus milk tea powder and preparation method thereof
CN106070861A (en) * 2016-06-06 2016-11-09 常立阁 A kind of compound Inonqqus obliquus alternative tea and preparation method thereof
CN107136262A (en) * 2017-05-19 2017-09-08 马永辉 One seed ginseng stilbene tea and its processing technology
CN112841493A (en) * 2021-02-22 2021-05-28 王奎 Inonotus obliquus solid beverage and preparation method thereof
CN116120480A (en) * 2023-01-06 2023-05-16 湖南杰萃生物技术有限公司 Method for simultaneously extracting inonotus obliquus polysaccharide and inonotus obliquus element
CN116120480B (en) * 2023-01-06 2024-04-26 湖南杰萃生物技术有限公司 Method for simultaneously extracting inonotus obliquus polysaccharide and inonotus obliquus element

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