CN102334685A - Preparation method of buckwheat flavone microcapsule and its product - Google Patents
Preparation method of buckwheat flavone microcapsule and its product Download PDFInfo
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Abstract
The invention provides a preparation method of a buckwheat flavone microcapsule, which comprises the following steps: 1) pretreating: drying buckwheat grain, buckwheat shell, buckwheat husk or buckwheat stem leaf, sieving after crushing for standby to obtain buckwheat powder; 2) extracting; 3) separating and purifying; 4) preparing a capsule emulsion: uniformly mixing a core material, a wall material and an emulsifier to prepare a buckwheat flavone microcapsule emulsion; 5) spray drying to obtain the buckwheat flavone microcapsule. The invention has the advantages that: 1, the activity of an active component flavone substance in buckwheat is protected; 2, the buckwheat flavone is prevented from damage of gastric acid, has certain targeting after microencapsulation, and has good enteric solubility but insolublility in stomach; 3, the bitter taste of buckwheat is covered; 4, the release speed is controlled, the flavone substance can not be stored in vivo, and the concentration of the flavone substance is rapidly increased in vivo after taking and rapidly decreasing due to metabolism degradation effect, the microencapsulation enables a slow release function and releases functional factors in certain time and scope.
Description
[technical field]
The present invention relates to preparation method of a kind of buckwheat flavonoids microcapsules and products thereof.
[background technology]
Modern medicine study finds that the flavonoids material is one of alimentary health-care function factor important in the buckwheat, and at shelled buckwheat, shell, stem, leaf, to spend middle ubiquity, its main component be rutin, content accounts for 70%～90% of general flavone.
Rutin has the effect of the capillary permeability of adjusting, can keep capillary resistance, reduce its permeability and fragility, and many-sided effect such as anti-inflammatory, diuresis, reducing blood lipid is arranged, clinically as capillary hemostatic, as the adjuvant therapy medicaments of vascular hypertension.Rutin is the primary raw material for preparing medicines such as monoxerutin, rutin tablets in the medical industry.Buckwheat aboundresources, seed mainly are as grain, and spend, leaf mainly is as medicine, comprehensive utilization, doctor's food homology can farthest be developed the value of natural products.
All contain abundant flavonoids material (being mainly rutin) in shelled buckwheat, shell, skin and the cauline leaf.Byproduct---buckwheat shell, skin and cauline leaf are casted away usually need not and buckwheat plantation produces.This is a huge waste beyond doubt, causes enormous economic loss to the peasant, and it is lower to add buckwheat preliminary working value-added content of product, therefore should strengthen the exploitation of buckwheat deep processed product as early as possible, buckwheat industry trend is become more meticulous and the high added value direction develops.
Along with science and technology development, the health-care effect of buckwheat and medical function are approved by everybody.The function factor of buckwheat is clear and definite; Function test also is gradually improved; Its Related product is except grain industry buckwheat rice, Buckwheat flour, noodles, bitter buckwheat tea, dustless buckwheat shell etc.; Also have the strong tea of the bitter buckwheat in " strong font size " product such as Lingqiu, Shanxi, the woman of " accurate font size " medicine such as sky, Shaanxi will medicine company puts down capsule, and products such as Beijing promise and the bitter buckwheat cellulose capsule of the international bio tech ltd new drug of all living creatures.Along with in recent years, people's living standard generally improves, and diabetes and cardiovascular and cerebrovascular patient are also more and more, especially America and Europe, Japan and Southeast Asia and China.Rutin is as the essential basic material medicine of treatment cardiovascular and cerebrovascular diseases, and the domestic and international market is all in short supply at present, and price per ton is between 15～170,000 yuan.Along with the appearance of Troxerutin standard, demand also continues to increase.Can affirm, quite grow one period, all vast market can be arranged both at home and abroad from now on.The deep level development of buckwheat has demonstrated great potential, and it is fully utilized is an industry with great economic benefit, is to revitalize China's local economy, particularly economic important channel, bitter cold remote districts.And at present, though buckwheat is regarded as treasure by many countries, really do not developed in China, the formation industry, and the processing level is lower, does not reach its height to tire, and competitiveness is not strong. alwaysCurrent, buckwheat processing enterprise utilizes shelled buckwheat, is processed into buckwheat, dried buckwheat noodle, buckwheat instant noodles, buckwheat vinegar etc. to shelled buckwheat.And a large amount of buckwheat shells, skin and cauline leaf almost do not utilize, and have only few part as pillow charges or fertilizer.In order to develop this kind of plant, be necessary its contained physiologically active ingredient flavonoids is carried out deep development and use.If buckwheat is carried out deep processing, process health products, just can improve capacity to earn foreign exchange through exports greatly.It is thus clear that the comprehensive utilization of buckwheat, the particularly developmental research of health products aspect are the important topics of buckwheat deep processing.
At present, flavonoids in the buckwheat is extracted the experimental study stage that still is in.Because flavonoids mostly is pure soluble substance, meets shipwreck and dissolve, and strong bitter taste is arranged.It directly is used for functional health-care food, not only be difficult to food in other compositions evenly mix, and can have a strong impact on the local flavor and the mouthfeel of product.
[summary of the invention]
The object of the present invention is to provide preparation method of a kind of buckwheat flavonoids microcapsules and products thereof, the product of this method preparation does not have bitter taste, easy to use.
To achieve these goals, the present invention adopts following technical scheme:
1, a kind of preparation method of buckwheat flavonoids microcapsules may further comprise the steps:
1) preliminary treatment:
Shelled buckwheat, buckwheat shell, buckwheat skin or buckwheat cauline leaf are crossed 40～60 mesh sieves after 60 ℃～80 ℃ oven dry, pulverizing subsequent use, gets buckwheat class powder;
2) extract:
Extract and make flavonoids in the buckwheat class powder in the step 1), get buckwheat flavonoids extract;
3) separation and purification:
To step 2) the buckwheat flavonoids extract that extracts carries out separation and purification, crude flavonoid powder;
4) capsule emulsion configuration:
Step 3) is made crude flavonoid powder be dissolved in the absolute ethyl alcohol, processing saturation classes flavones ethanol solution is core; Core, wall material and emulsifier is even, make buckwheat flavonoids microcapsule emulsion; Wherein, the mass ratio of core and wall material is 1: (6～9); Emulsifying agent accounts for 0.3%～0.5% of wall material amount;
Said wall material is 1 by mass ratio: the soybean protein isolate solution and the ethyl cellulose solution of (3～5) are formed; Said soybean protein isolate solution is water-soluble formulated by soybean protein isolate, and its mass concentration is 15%; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%;
Perhaps said wall material is made up of the gumwater and the ethyl cellulose solution of saturated beta-schardinger dextrin-solution, mass concentration 10%; The quality percentage composition that said saturated beta-schardinger dextrin-solution, the gumwater of mass concentration 10%, ethyl cellulose solution account for the wall material is respectively 40%～70%, 25%～55%, 5%～35%; Said saturated beta-schardinger dextrin-solution is water-soluble formulated by beta-schardinger dextrin-; Said mass concentration is that 10% gumwater is water-soluble formulated by Arabic gum; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%;
Perhaps said wall material is made up of the gumwater and the ethyl cellulose solution of dextrin solution, mass concentration 10%; The quality percentage composition that the gumwater of said dextrin solution, mass concentration 10%, ethyl cellulose solution account for the wall material is respectively 0%～50%, 20%～50%, 30%～60%; Said mass concentration is that 10% gumwater is water-soluble formulated by Arabic gum; Said dextrin solution is water-soluble formulated by dextrin, and its mass concentration is 10%; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%;
Said emulsifying agent is a monoglyceride solution, and it is water-soluble formulated by monoglyceride, and its mass concentration is 15%;
5) spray-drying:
Step 4) gained buckwheat flavonoids microcapsule emulsion is carried out spray-drying, get buckwheat flavonoids microcapsules.
The present invention further improves and is: extracting and making the method that flavonoids adopted in the buckwheat class powder in the step 1) is the auxiliary organic solvent method of ultrasonic wave or biological enzyme-ultrasonic wave combined techniques; The organic solvent that adopts in the auxiliary organic solvent method of ultrasonic wave is that volumetric concentration is 40～70% ethanolic solution.
The present invention further improves and is: the mass ratio of said core and wall material is 3: 22; Said wall material is that 1: 4 soybean protein isolate solution and ethyl cellulose solution formed by mass ratio; Said soybean protein isolate solution is water-soluble formulated by soybean protein isolate, and its mass concentration is 15%; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%; Emulsifying agent accounts for 0.5% of wall material amount;
The step of said step 4) is: with saturation classes flavones ethanol solution and ethyl cellulose solution and emulsifier; Under rotating speed 1500～1800r/min, stir; Be distributed to then in 40～60 ℃ the soybean protein isolate solution; Control then and be cooled to room temperature rotating speed stirs 5～10min under 500～800r/min after, obtain buckwheat flavonoids microcapsule emulsion.
The present invention further improves and is: the mass ratio of said core and wall material is 1: 9; Said wall material is made up of the gumwater and the ethyl cellulose solution of saturated beta-schardinger dextrin-solution, mass concentration 10%; The quality percentage composition that said saturated beta-schardinger dextrin-solution, the gumwater of mass concentration 10%, ethyl cellulose solution account for the wall material is respectively 51.88%, 35.29%, 12.83%; Said saturated beta-schardinger dextrin-solution is water-soluble formulated by beta-schardinger dextrin-; Said mass concentration is that 10% gumwater is water-soluble formulated by Arabic gum; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%; The emulsifying agent addition is 0.5% of a wall material amount;
The step of said step 4) is: saturation classes flavones ethanol solution is added saturated beta-schardinger dextrin-solution; Under 500～800r/min, stir; Add mass concentration 10% gumwater and emulsifying agent then, after continuing to stir 5～10min, add ethyl cellulose solution again; Under 1500～1800r/min, stir 5～8min, obtain buckwheat flavonoids microcapsule emulsion.
The present invention further improves and is: the mass ratio of said core and wall material is 3: 22; Said wall material is by being made up of the gumwater and the ethyl cellulose solution of dextrin solution, mass concentration 10%; The quality percentage composition that the gumwater of said dextrin solution, mass concentration 10%, ethyl cellulose solution account for the wall material is respectively 34.58%, 27.23%, 38.19%; Said mass concentration is that 10% gumwater is water-soluble formulated by Arabic gum; Said dextrin solution is water-soluble formulated by dextrin, and its mass concentration is 10%; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%; The emulsifying agent addition is 0.4% of a wall material amount;
The step of said step 4) is: with the gumwater of saturation classes flavones ethanol solution and emulsifying agent adding mass concentration 10%; Under rotating speed 500～800r/min, stir; Add dextrin solution and ethyl cellulose solution then; Under 1500～1800r/min, stir 5～8min, obtain buckwheat flavonoids microcapsule emulsion.
The present invention further improves and is: adopt macroporous absorbent resin to carry out separation and purification in the step 3); The model of said macroporous absorbent resin is AB-8, HPD100 or XDA-5.
The present invention further improves and is: biological enzyme-ultrasonic wave combined techniques may further comprise the steps: is 1 with buckwheat class powder according to solid-liquid ratio: (30～50) g/mL adds in the combination enzyme solutions; PH value 4.0～5.0; 30～50 ℃ of hydrolysis temperatures, the ultrasonic wave enzyme is handled 40～80min; Wherein make up and comprise cellulase, 1,4 beta-glucanase and zytase in the enzyme solutions; Cellulase activity >=400,000 u/g, activity of beta-glucanase >=3,000,000 u/g, Xylanase activity >=2,600,000 u/g.
The present invention further improves and is: the spray-dired condition of step 5) is: 60～80 ℃ of buckwheat flavonoids microcapsule emulsion temperature; Sample introduction flow velocity 15～30mL/min; Centrifugal rotational speed 18000～24000r/min, 150～180 ℃ of intake air temperatures, 60～80 ℃ of air outlet temperature.
The present invention further improves and is: the spray-dired condition of step 5) is: 60 ℃ of buckwheat flavonoids microcapsule emulsion temperature, sample introduction flow velocity 20mL/min, rotating speed 24000r/min, 160 ℃ of intake air temperatures, 80 ℃ of air outlet temperature.
Compared with prior art, the present invention has the following advantages:
1, the activity of active component flavonoids material in the protection buckwheat; 2, protection buckwheat flavonoids is by stomach acids destroy, and generally in intestines, just is absorbed, and can have certain target property behind the microencapsulation, and stomach is insoluble and enteric solubility is good; 3, cover the buckwheat bitter taste; 4, control rate of release; The flavonoids material can not be stored in vivo, and edible back concentration rises rapidly in vivo, reduces rapidly owing to the metabolic degradation effect afterwards; Microencapsulation can make it to have slow-release function, the stable function factor that discharges in the certain hour scope; 5, increase usefulness; Because water-soluble extremely low and the photo-thermal acid labile of buckwheat flavonoids have limited its purposes, microencapsulation can well address this problem; Simultaneously can increase its mechanical strength again, make it to be applied to better more easily health care of food article, medicine etc. multi-field in.
[specific embodiment]
Below with specific embodiment technology of preparing scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1
The shelled buckwheat flavonoids microcapsules of present embodiment, the treatment technology route that comprises are that the auxiliary organic solvent method of ultrasonic wave extracts, macroreticular resin separates and purifying buckwheat flavonoids, and the microcapsule embedded and spray-drying flavonoids microencapsulation of flavonoids is handled.
The flavonoids microcapsule preparation method of present embodiment may further comprise the steps:
(1) preliminary treatment: shelled buckwheat is pulverized after 60 ℃ of oven dry, crossed 60 mesh sieves, it is subsequent use to get the shelled buckwheat powder;
(2) extract: is 1 with the shelled buckwheat powder according to solid-liquid ratio: it is in 40% the ethanolic solution that the ratio of 20g/mL adds volumetric concentration; Place the Extraction by Ultrasound device; Ultrasonic power is 160W; 65 ℃ of temperature, Extraction by Ultrasound 41min gets shelled buckwheat flavonoids extract to extract the flavonoids in the shelled buckwheat;
(3) separation and purification: continuously through being filled with the adsorption column of macroporous absorbent resin, target component is stayed in the adsorption column shelled buckwheat flavonoids extract; The macroporous absorbent resin model is AB-8, and shelled buckwheat flavonoids extract concentration is 0.32mg/mL, upper column quantity 7BV, absorption flow velocity 2.0mL/min; By the buckwheat flavonoids of macroporous absorbent resin absorption, stripping liquid employing volumetric concentration is 40% ethanol, desorb flow velocity 1.5mL/min, stripping liquid consumption 100mL with the stripping liquid wash-out; The eluent of collecting is carried out condensing crystallizing, obtain the crude flavonoid powder sample;
(4) microcapsules preparation: at first the crude flavonoid powder sample ligand is processed saturation classes flavones ethanol solution as core with absolute ethyl alcohol; The wall material is made up of mass ratio 1: 4 soybean protein isolate solution and ethyl cellulose solution; Emulsifying agent is a monoglyceride solution, and the emulsifying agent addition is 0.5% of a wall material amount; Press 3: 22 core wall proportioning of mass ratio then; Core solution is fully mixed with ethyl cellulose solution and emulsifying agent monoglyceride solution; Under rotating speed 1800r/min, stir; Be distributed to rapidly then in 50 ℃ the soybean protein isolate solution, control rate is cooled to room temperature and obtains buckwheat flavonoids microcapsule emulsion after 800r/min stirs 8min; Above-mentioned soybean protein isolate solution is water-soluble formulated by soybean protein isolate, and its mass concentration is 15%; It is formulated that above-mentioned ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%; Above-mentioned monoglyceride solution is water-soluble formulated by monoglyceride, and its mass concentration is 15%;
(5) spray-drying: the buckwheat flavonoids microcapsule emulsion that step (4) is obtained is carried out spray-drying with spray dryer and is processed buckwheat flavonoids microcapsules; Spray-dired condition is: 60 ℃ of buckwheat flavonoids microcapsule emulsion temperature, sample introduction flow velocity 20mL/min, rotating speed 24000r/min, 160 ℃ of intake air temperatures, 80 ℃ of air outlet temperature.
Embodiment 2
The buckwheat shell flavonoids microcapsules of present embodiment, the treatment technology route that comprises are that the auxiliary organic solvent method of ultrasonic wave extracts, macroreticular resin separates and purifying buckwheat flavonoids, and the microcapsule embedded and spray-drying flavonoids microencapsulation of flavonoids is handled.
The flavonoids microcapsule preparation method of present embodiment may further comprise the steps:
(1) preliminary treatment: buckwheat shell is pulverized after 60 ℃ of oven dry, crosses 40 mesh sieves, and it is subsequent use to get the buckwheat shell powder;
(2) extract: is 1 with the buckwheat shell powder according to solid-liquid ratio: it is in 40% the ethanolic solution that the ratio of 47g/mL adds volumetric concentration; Place the Extraction by Ultrasound device; Ultrasonic power 195W; 70 ℃ of temperature, Extraction by Ultrasound 70min gets buckwheat shell flavonoids extract to extract the flavonoids in the buckwheat shell;
(3) separation and purification: continuously through being filled with the adsorption column of macroporous absorbent resin, target component is stayed in the adsorption column buckwheat shell flavonoids extract; The macroporous absorbent resin model is AB-8, and buckwheat shell flavonoids extract concentration is 0.24mg/mL, upper column quantity 8BV, absorption flow velocity 2.0mL/min; By the buckwheat flavonoids of macroporous absorbent resin absorption, stripping liquid employing volumetric concentration is 40% ethanol, desorb flow velocity 1.0mL/min, stripping liquid consumption 100mL with the stripping liquid wash-out; The eluent of collecting is carried out condensing crystallizing, obtain the crude flavonoid powder sample;
(4) microcapsules preparation: at first prepare core and wall material, the mass ratio of core and wall material is 1: 9; Core is the saturation classes flavones ethanol solution that the crude flavonoid powder sample of step (3) separation and purification forms with the absolute ethyl alcohol configuration; The wall material is a compound wall materials, and it comprises that saturated beta-schardinger dextrin-solution, mass concentration are 3 kinds of raw materials of gumwater, ethyl cellulose solution of 10%, and 3 kinds of raw materials mass fraction of shared compound wall materials separately are 51.88%, 35.29%, 12.83%; At first; Saturated core solution is added in the saturated beta-schardinger dextrin-solution; After under 800r/min, stirring, adding mass concentration then is 10% gumwater and emulsifying agent monoglyceride, after continuing to stir 10min; Slowly add ethyl cellulose solution, under 1800r/min, stir 8min and obtain buckwheat flavonoids microcapsule emulsion; The emulsifying agent addition is 0.5% of a wall material amount; Above-mentioned saturated beta-schardinger dextrin-solution is water-soluble formulated by beta-schardinger dextrin-; Above-mentioned mass concentration is that 10% gumwater is water-soluble formulated by Arabic gum; It is formulated that above-mentioned ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%; Above-mentioned monoglyceride solution is water-soluble formulated by monoglyceride, and its mass concentration is 15%;
(5) spray-drying: the buckwheat flavonoids microcapsule emulsion that step (4) is obtained is carried out spray-drying with spray dryer and is processed buckwheat flavonoids microcapsules; Spray-dired condition is: 60 ℃ of emulsion temperature, sample introduction flow velocity 20mL/min, rotating speed 24000r/min, 160 ℃ of intake air temperatures, 80 ℃ of air outlet temperature.
Embodiment 3
The buckwheat skin flavonoids microcapsules of present embodiment, the treatment technology route that comprises are that biological enzyme-ultrasonic wave combined techniques extracts, macroreticular resin separates and purifying buckwheat flavonoids, and the microcapsule embedded and spray-drying flavonoids microencapsulation of flavonoids is handled.
The flavonoids microcapsule preparation method of present embodiment may further comprise the steps:
(1) preliminary treatment: buckwheat skin is pulverized after 60 ℃ of oven dry, crosses 60 mesh sieves, and it is subsequent use to get the buckwheat skin powder;
(2) extract: is 1 with the buckwheat skin powder according to solid-liquid ratio: 45g/ml adds in the composite enzyme solution, and composite enzyme solution consists of cellulase (enzyme activity >=400,000 u/g), 1,4 beta-glucanase (enzyme activity >=3,000,000 u/g), zytase (enzyme activity >=2,600,000 u/g); Enzyme concentration is 0.54mg/mL in the composite enzyme solution, pH value 4.6, and 40 ℃ of hydrolysis temperatures are behind the enzyme processing time 71min; Under ultrasonic power 125W, handle 30min, get buckwheat skin flavonoids extract;
(3) separation and purification: continuously through being filled with the adsorption column of macroporous absorbent resin, target component is stayed in the adsorption column buckwheat skin flavonoids extract; The model HPD100 of macroporous absorbent resin, absorption flow velocity 1.0mL/min, maximum applied sample amount 10BV, sample solution concentration 0.5mg/mL; By the buckwheat flavonoids of macroporous absorbent resin absorption, stripping liquid is that volumetric concentration is 60% ethanolic solution, stripping liquid flow velocity 1.0mL/min, stripping liquid consumption 100mL with the stripping liquid wash-out; Collect eluent, the eluent of collecting is carried out condensing crystallizing, obtain the crude flavonoid powder sample;
(4) microcapsules preparation: at first prepare core and wall material, adopt the crude flavonoid powder sample to be mixed with saturation classes flavones ethanol solution as core with absolute ethyl alcohol; The mass ratio of core and wall material is 3: 22; The wall material is a compound wall materials, and compound wall materials is made up of gumwater, dextrin solution, the ethyl cellulose solution of mass concentration 10%, and the mass percent of shared compound wall materials is 27.23%, 34.58%, 38.19% separately; During preparation; The gumwater that at first saturated buckwheat flavonoids solution and the emulsifying agent monoglyceride solution that accounts for wall material amount 0.4% is added mass concentration 10%; After rotating speed 800r/min stirs; Add dextrin solution and ethyl cellulose solution then, under 1800r/min, stir 8min and get buckwheat flavonoids microcapsule emulsion; Above-mentioned mass concentration is that 10% gumwater is water-soluble formulated by Arabic gum; Above-mentioned dextrin solution is water-soluble formulated by dextrin, and its mass concentration is 10%; It is formulated that above-mentioned ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%; Above-mentioned monoglyceride solution is water-soluble formulated by monoglyceride, and its mass concentration is 15%;
(5) spray-drying: the buckwheat flavonoids microcapsule emulsion that step (4) is obtained is carried out spray-drying with spray dryer and is processed buckwheat flavonoids microcapsules; Spray-dired condition is: 60 ℃ of emulsion temperature, sample introduction flow velocity 20mL/min, rotating speed 24000r/min, 180 ℃ of intake air temperatures, 80 ℃ of air outlet temperature.
Embodiment 4
The buckwheat cauline leaf flavonoids microcapsules of present embodiment, the treatment technology route that comprises are that organic solvent method extracts, macroreticular resin separates and purifying buckwheat flavonoids, and the microcapsule embedded and spray-drying flavonoids microencapsulation of flavonoids is handled.
The flavonoids microcapsule preparation method of present embodiment may further comprise the steps:
(1) preliminary treatment: the buckwheat cauline leaf is pulverized after 80 ℃ of oven dry, crosses 40 mesh sieves, and it is subsequent use to get buckwheat cauline leaf powder;
(2) extract: is 1 with buckwheat cauline leaf powder according to solid-liquid ratio: the ratio of 40g/mL adds volumetric concentration to be in 70% the ethanolic solution and to mix; Place the Extraction by Ultrasound device; Ultrasonic power 175W; 75 ℃ of temperature, Extraction by Ultrasound 2.0h gets buckwheat cauline leaf flavonoids extract to extract the flavonoids in the buckwheat cauline leaf;
(3) separation and purification: continuously through being filled with the adsorption column of macroporous absorbent resin, target component is stayed in the adsorption column buckwheat cauline leaf flavonoids extract; Macroreticular resin model XDA-5, adsorption liquid concentration 0.16mg/mL, upper column quantity 11BV, absorption flow velocity 2.0mL/min; By the buckwheat flavonoids of macroporous absorbent resin absorption, stripping liquid employing volume fraction is 80% ethanolic solution, desorb flow velocity 1.0mL/min, stripping liquid consumption 100mL with the stripping liquid wash-out; The eluent of collecting is carried out condensing crystallizing, obtain the crude flavonoid powder sample;
(4) microcapsules preparation: at first prepare core and wall material; Adopt the crude flavonoid powder sample to be mixed with saturation classes flavones ethanol solution as core with absolute ethyl alcohol; The mass ratio of core and wall material is 3: 22; The wall material is that 1: 4 soybean protein isolate solution and ethyl cellulose solution formed by mass ratio, and the addition of emulsifying agent monoglyceride solution is a wall material amount 0.5%; During preparation; At first core solution and ethyl cellulose solution and emulsifying agent monoglyceride solution are fully mixed; Under rotating speed 1800r/min, be distributed to rapidly in 50 ℃ the soybean protein isolate solution, control rate stirs under 800r/min and is cooled to room temperature behind the 8min and obtains buckwheat flavonoids microcapsule emulsion; Above-mentioned soybean protein isolate solution is water-soluble formulated by soybean protein isolate, and its mass concentration is 15%; It is formulated that above-mentioned ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%; Above-mentioned monoglyceride solution is water-soluble formulated by monoglyceride, and its mass concentration is 15%;
(5) spray-drying: the buckwheat flavonoids microcapsule emulsion that step (4) is obtained is carried out spray-drying with spray dryer and is processed buckwheat flavonoids microcapsules; Spray-dired condition is: 60 ℃ of emulsion temperature, sample introduction flow velocity 20mL/min, rotating speed 24000r/min, 180 ℃ of intake air temperatures, 80 ℃ of air outlet temperature.
Spray-drying of the present invention adopts the cis centrifugal spray drying tower.
Buckwheat flavonoids microcapsules behind the spray drying forming can carry out quantitative package as required, are used widely as functional food, health products auxiliary material or medicine base-material, also may be used on other field.
The best purification condition of shelled buckwheat flavonoids is the AB-8 macroreticular resin among the present invention, adsorption liquid concentration 0.32mg/mL, upper column quantity 7BV, absorption flow velocity 2.0mL/min, stripping liquid concentration 40%, desorb flow velocity 1.5mL/min; The best purification condition of buckwheat shell flavonoids is the AB-8 macroreticular resin, adsorption liquid concentration 0.24mg/mL, upper column quantity 8BV, absorption flow velocity 2.0mL/min, stripping liquid concentration 40%, desorb flow velocity 1.0mL/min; Buckwheat skin flavonoids optimum process condition is the HPD100 macroreticular resin, and the absorption flow velocity is 1mL/min, and maximum applied sample amount is 10BV, and sample solution concentration is 0.5mg/mL, and the strippant volume fraction is 60%, and the strippant flow velocity is 1mL/min, and the strippant consumption is 6BV; The best purification condition of buckwheat cauline leaf flavonoids is the XDA-5 macroreticular resin, adsorption liquid concentration 0.16mg/mL, upper column quantity 11BV, absorption flow velocity 2.0mL/min, stripping liquid concentration 80%, desorb flow velocity 1.0mL/min.
Buckwheat flavonoids of the present invention carries out microencapsulation, and through the flavonoids microcapsules microcapsule embedded, that drying makes, greatly expansion of range of application, processing characteristics and physiologically active significantly improve; When microcapsule embedded; Adopting soybean protein-ethyl cellulose embedding buckwheat flavonoids optimum process condition is that core wall mass ratio is 3: 22, and temperature is 50 ℃, and the monoglyceride addition is a wall material amount 0.5%; The wall material consists of soybean protein and ethyl cellulose, and mass fraction is respectively 25% and 75%; Beta-schardinger dextrin--Arabic gum-ethyl cellulose embedding buckwheat flavonoids optimum process condition is core wall mass ratio 1: 9; The emulsifying agent addition is 0.3% of a wall material amount; The wall material consists of beta-schardinger dextrin-51.88%, Arabic gum 35.29%, ethyl cellulose 12.83% by mass percent; The optimum process condition of Arabic gum-dextrin-ethyl cellulose embedding buckwheat flavonoids is core wall mass ratio 3: 22; The emulsifying agent addition is a wall material amount 0.4%, and the wall material consists of ethyl cellulose 38.19%, Arabic gum 27.23% and dextrin 34.58% by mass percent; Microcapsules drying process with atomizing condition is 60 ℃ of emulsion temperature, sample introduction flow velocity 20mL/min, rotating speed 24000r/min, 160 ℃ of intake air temperatures, 80 ℃ of air outlet temperature.Above-mentioned buckwheat flavonoids is a flavonoids in shelled buckwheat, shell, skin and the cauline leaf.
The present invention carries out microencapsulation to the flavonoids material, and a variety of inorganic material and organic material are all as the wall material, but a kind of material is difficult to reach requirement, and the present invention adopts several kinds of compound uses of wall material.The present invention adopts ethyl cellulose to make the flavonoids microcapsule wall material, and it has thermoplasticity and water-insoluble, Heat stability is good; The adhesion sense is seldom arranged or send out puckery, can generate tough and tensile film, nontoxic; Extremely strong antibiont performance is arranged; Prepare slow-release microcapsule as the packing auxiliary material, make drug effect continue to discharge, avoid some water soluble drugs to have an effect too early; Simultaneously ethyl cellulose is as stable, functional, nontoxic, safe microencapsulation wall material, prepares at microcapsules to show its unique advantages in the process.
The present invention is with functional components flavonoids microencapsulation, and the activity of preserving core to greatest extent reduces the influence of extraneous undesirable element; Control the release of core, cover the peculiar smell of heartwood, change physicochemical properties and the light sensitivity and the thermal sensitivity of heartwood; Improve the operability of core; Make it to have excellent function character and bin stability, can more conveniently be applied to industries such as food medicine widely, solve the problem that traditional handicraft institute can not or be difficult to solution.It is thus clear that the present invention has advanced technical and more wide application prospect, the deep processing development utilization that can be buckwheat provides technical support.
The buckwheat flavonoids has multiple pharmacological effect and health function, but buckwheat shell, skin and cauline leaf fail to be fully used in buckwheat deep processing and utilization process, cause the wasting of resources of certain degree.The present invention extracts the flavonoids in preparation shelled buckwheat, shell, skin and the cauline leaf through biological and physical method, and behind macroporous resin purification, after the micro capsule technology embedding, the buckwheat flavonoids microcapsules that spray-dried again powder process obtains; Existing good sense organ, processing characteristics have good masking protection, slow-release function again, give full play to the medicinal health function of buckwheat flavonoids, enlarge its range of application.Buckwheat flavonoids microcapsules of the present invention are convenient to storage, transport and as base-material interpolation, use, have been improved the added value of buckwheat flavonoids, for the economic development of producing the buckwheat district provides new thinking.Therefore, the present invention has good society and economic worth, is easy to apply.
Be noted that at last: above embodiment is the unrestricted technology of preparing scheme of the present invention in order to explanation only; Although the present invention is specified with reference to the foregoing description; But as it should be appreciated by those skilled in the art: still can make amendment or be equal to replacement to the present invention; And not breaking away from any modification or the localized variation of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (10)
1. the preparation method of buckwheat flavonoids microcapsules is characterized in that, may further comprise the steps:
1) preliminary treatment:
Shelled buckwheat, buckwheat shell, buckwheat skin or buckwheat cauline leaf are crossed 40～60 mesh sieves after 60 ℃～80 ℃ oven dry, pulverizing subsequent use, gets buckwheat class powder;
2) extract:
Extract and make flavonoids in the buckwheat class powder in the step 1), get buckwheat flavonoids extract;
3) separation and purification:
To step 2) the buckwheat flavonoids extract that extracts carries out separation and purification, crude flavonoid powder;
4) capsule emulsion configuration:
Step 3) is made crude flavonoid powder be dissolved in the absolute ethyl alcohol, processing saturation classes flavones ethanol solution is core; Core, wall material and emulsifier is even, make buckwheat flavonoids microcapsule emulsion; Wherein, the mass ratio of core and wall material is 1: (6～9); Emulsifying agent accounts for 0.3%～0.5% of wall material amount;
Said emulsifying agent is a monoglyceride solution, and it is water-soluble formulated by monoglyceride, and its mass concentration is 15%;
Said wall material is 1 by mass ratio: the soybean protein isolate solution and the ethyl cellulose solution of (3～5) are formed; Said soybean protein isolate solution is water-soluble formulated by soybean protein isolate, and its mass concentration is 15%; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%;
Perhaps said wall material is made up of the gumwater and the ethyl cellulose solution of saturated beta-schardinger dextrin-solution, mass concentration 10%; The quality percentage composition that said saturated beta-schardinger dextrin-solution, the gumwater of mass concentration 10%, ethyl cellulose solution account for the wall material is respectively 40%～70%, 25%～55%, 5%～35%; Said saturated beta-schardinger dextrin-solution is water-soluble formulated by beta-schardinger dextrin-; Said mass concentration is that 10% gumwater is water-soluble formulated by Arabic gum; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%;
Perhaps said wall material is made up of the gumwater and the ethyl cellulose solution of dextrin solution, mass concentration 10%; The quality percentage composition that the gumwater of said dextrin solution, mass concentration 10%, ethyl cellulose solution account for the wall material is respectively 0%～50%, 20%～50%, 30%～60%; Said mass concentration is that 10% gumwater is water-soluble formulated by Arabic gum; Said dextrin solution is water-soluble formulated by dextrin, and its mass concentration is 10%; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%;
5) spray-drying:
Step 4) gained buckwheat flavonoids microcapsule emulsion is carried out spray-drying, get buckwheat flavonoids microcapsules.
2. a kind of according to claim 1 preparation method of buckwheat flavonoids microcapsules is characterized in that, extracting and making the method that flavonoids adopted in the buckwheat class powder in the step 1) is the auxiliary organic solvent method of ultrasonic wave or biological enzyme-ultrasonic wave combined techniques; The organic solvent that adopts in the auxiliary organic solvent method of ultrasonic wave is that volumetric concentration is 40～70% ethanolic solution.
3. a kind of according to claim 1 preparation method of buckwheat flavonoids microcapsules is characterized in that, the mass ratio of said core and wall material is 3: 22; Said wall material is that 1: 4 soybean protein isolate solution and ethyl cellulose solution formed by mass ratio; Said soybean protein isolate solution is water-soluble formulated by soybean protein isolate, and its mass concentration is 15%; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%; Emulsifying agent accounts for 0.5% of wall material amount;
The step of said step 4) is: with saturation classes flavones ethanol solution and ethyl cellulose solution and emulsifier; Under rotating speed 1500～1800r/min, stir; Be distributed to then in 40～60 ℃ the soybean protein isolate solution; Control then and be cooled to room temperature rotating speed stirs 5～10min under 500～800r/min after, obtain buckwheat flavonoids microcapsule emulsion.
4. a kind of according to claim 1 preparation method of buckwheat flavonoids microcapsules is characterized in that, the mass ratio of said core and wall material is 1: 9; Said wall material is made up of the gumwater and the ethyl cellulose solution of saturated beta-schardinger dextrin-solution, mass concentration 10%; The quality percentage composition that said saturated beta-schardinger dextrin-solution, the gumwater of mass concentration 10%, ethyl cellulose solution account for the wall material is respectively 51.88%, 35.29%, 12.83%; Said saturated beta-schardinger dextrin-solution is water-soluble formulated by beta-schardinger dextrin-; Said mass concentration is that 10% gumwater is water-soluble formulated by Arabic gum; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%; The emulsifying agent addition is 0.5% of a wall material amount;
The step of said step 4) is: saturation classes flavones ethanol solution is added saturated beta-schardinger dextrin-solution; Under 500～800r/min, stir; Add mass concentration 10% gumwater and emulsifying agent then, after continuing to stir 5～10min, add ethyl cellulose solution again; Under 1500～1800r/min, stir 5～8min, obtain buckwheat flavonoids microcapsule emulsion.
5. a kind of according to claim 1 preparation method of buckwheat flavonoids microcapsules is characterized in that, the mass ratio of said core and wall material is 3: 22; Said wall material is by being made up of the gumwater and the ethyl cellulose solution of dextrin solution, mass concentration 10%; The quality percentage composition that the gumwater of said dextrin solution, mass concentration 10%, ethyl cellulose solution account for the wall material is respectively 34.58%, 27.23%, 38.19%; Said mass concentration is that 10% gumwater is water-soluble formulated by Arabic gum; Said dextrin solution is water-soluble formulated by dextrin, and its mass concentration is 10%; It is formulated that said ethyl cellulose solution is dissolved in absolute ethyl alcohol by ethyl cellulose, and its mass concentration is 30%; The emulsifying agent addition is 0.4% of a wall material amount;
The step of said step 4) is: with the gumwater of saturation classes flavones ethanol solution and emulsifying agent adding mass concentration 10%; Under rotating speed 500～800r/min, stir; Add dextrin solution and ethyl cellulose solution then; Under 1500～1800r/min, stir 5～8min, obtain buckwheat flavonoids microcapsule emulsion.
6. a kind of according to claim 1 preparation method of buckwheat flavonoids microcapsules is characterized in that, adopts macroporous absorbent resin to carry out separation and purification in the step 3); The model of said macroporous absorbent resin is AB-8, HPD100 or XDA-5.
7. like the preparation method of the said a kind of buckwheat flavonoids microcapsules of claim 2; It is characterized in that; Biological enzyme-ultrasonic wave combined techniques may further comprise the steps: is 1 with buckwheat class powder according to solid-liquid ratio: (30～50) g/mL adds in the combination enzyme solutions; PH value 4.0～5.0,30～50 ℃ of hydrolysis temperatures, the ultrasonic wave enzyme is handled 40～80min; Wherein make up and comprise cellulase, 1,4 beta-glucanase and zytase in the enzyme solutions; Cellulase activity >=400,000 u/g, activity of beta-glucanase >=3,000,000 u/g, Xylanase activity >=2,600,000 u/g.
8. a kind of according to claim 1 preparation method of buckwheat flavonoids microcapsules; It is characterized in that; The spray-dired condition of step 5) is: 60～80 ℃ of buckwheat flavonoids microcapsule emulsion temperature, sample introduction flow velocity 15～30mL/min, centrifugal rotational speed 18000～24000r/min; 150～180 ℃ of intake air temperatures, 60～80 ℃ of air outlet temperature.
9. like the preparation method of the said a kind of buckwheat flavonoids microcapsules of claim 8, it is characterized in that the spray-dired condition of step 5) is: 60 ℃ of buckwheat flavonoids microcapsule emulsion temperature; Sample introduction flow velocity 20mL/min; Rotating speed 24000r/min, 160 ℃ of intake air temperatures, 80 ℃ of air outlet temperature.
10. the product that makes by the preparation method of each said a kind of buckwheat flavonoids microcapsules among the claim 1-9.
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| CN103446254A (en) * | 2013-08-13 | 2013-12-18 | 西北大学 | Embedding method of buckwheat flavonoids |
| CN104825551B (en) * | 2015-05-15 | 2018-05-29 | 吉林农业大学 | A kind of buckwheat shell chromocor extract and application |
| CN104825551A (en) * | 2015-05-15 | 2015-08-12 | 吉林农业大学 | Buckwheat shell flavonoid extract and application thereof |
| CN105238098A (en) * | 2015-11-02 | 2016-01-13 | 江苏食品药品职业技术学院 | Dynamic gradient embedding method for purple corn cob anthocyanin |
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