CN106579450B - Gynostemma pentaphylla seed fatty acid microcapsule and preparation method and application thereof - Google Patents
Gynostemma pentaphylla seed fatty acid microcapsule and preparation method and application thereof Download PDFInfo
- Publication number
- CN106579450B CN106579450B CN201611092316.3A CN201611092316A CN106579450B CN 106579450 B CN106579450 B CN 106579450B CN 201611092316 A CN201611092316 A CN 201611092316A CN 106579450 B CN106579450 B CN 106579450B
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- Prior art keywords
- gynostemma pentaphylla
- fatty acid
- pentaphylla seed
- solution
- preparation
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Abstract
The invention relates to a gynostemma pentaphylla seed fatty acid microcapsule, a preparation method and application thereof, wherein maltodextrin, soybean protein isolate and gynostemma pentaphylla seed aqueous extract are firstly taken to be dissolved in water and uniformly mixed to form a wall material phase solution; adding the gynostemma pentaphylla seed fatty acid into the composite emulsifier solution to form a core material phase solution; mixing the wall material phase solution and the core material phase solution, and uniformly stirring to obtain a mixed solution; in the mixed solution, by mass percent, 10-15% of maltodextrin, 5-10% of soybean protein isolate, 5-10% of gynostemma pentaphylla seed water extract, 10-15% of gynostemma pentaphylla seed fatty acid and 1.7-3.5% of a composite emulsifier are added; and sequentially carrying out primary emulsification, homogenization treatment and freeze drying on the mixed solution to obtain the gynostemma pentaphylla seed fatty acid microcapsule. The raw materials of the invention are widely available, and the prepared microcapsule has stable performance, long shelf life and good biological activity, is not easy to be oxidized, and can be applied to the preparation of anti-tumor and blood fat-reducing medicines.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the field of microcapsule preparation, and particularly relates to a gynostemma pentaphylla seed fatty acid microcapsule, and a preparation method and application thereof.
[ background of the invention ]
Gynostemma pentaphylla (Gynostemma pentaphylum) is a perennial herbaceous vine plant of Cucurbitaceae, also called herba Picrasmae, radix Et caulis Acanthopanacis Senticosi, radix Panacis Quinquefolii, herba Gynostemmatis, radix seu folium Gynostemmatis, and radix ubiquitinae, and is mainly distributed in Qinling and south of Yangtze river in China, and is called as "south ginseng" and "second ginseng" because of the rich ginsenoside components in vivo. The oil content of the gynostemma pentaphylla seed is more than 40%, and the gynostemma pentaphylla seed can be comparable to rapeseed oil, and the main component of the gynostemma pentaphylla seed oil is fatty acid, while the gynostemma pentaphylla fatty acid is mainly conjugated linolenic acid and accounts for more than 90% of the total fatty acid.
The microcapsule technology is a technology of encapsulating solid, liquid or gas into a film-forming material to form a micro container with a diameter of several micrometers to thousands of micrometers, the material loaded inside the microcapsule is called a core material (or capsule core material), and the wall film encapsulated outside is called a wall material (or capsule material). After decades of continuous development, microcapsule technology has become mature, and is widely applied in the industrial fields of pharmacy, food, agricultural chemicals, spices, feed additives, daily chemicals and the like. Among them, the microcapsule technology is particularly interesting in the field of preparation of high value-added oil products. After microencapsulation, the heat sensitivity and photosensitivity of the grease are reduced, so that the fat-soluble components can be prevented from being damaged, and the nutrition, flavor stability and bioavailability of the grease product are improved.
At present, polyunsaturated fatty acid microencapsulation is generally carried out by adopting a high-temperature spray drying method, which has low cost, simple process and easy large-scale industrial production, but has high temperature required by evaporation, easy inactivation of active ingredients, easy gap on the capsule wall and poor compactness. Due to the fact that the fatty acid peroxide value of the gynostemma pentaphylla seeds is high, the risk of oxidation is increased due to the fact that the temperature is too high.
[ summary of the invention ]
The invention aims to overcome the problems in the prior art and provide the gynostemma pentaphylla seed fatty acid microcapsule as well as the preparation method and the application thereof.
The preparation method comprises the following technical scheme:
the method comprises the following steps:
(1) dissolving maltodextrin, soy protein isolate and gynostemma pentaphylla seed aqueous extract in water, and uniformly mixing to form a wall material phase solution;
(2) adding the gynostemma pentaphylla seed fatty acid into the composite emulsifier solution to form a core material phase solution;
(3) mixing the wall material phase solution and the core material phase solution, and uniformly stirring to obtain a mixed solution; in the mixed solution, by mass percent, 10-15% of maltodextrin, 5-10% of soybean protein isolate, 5-10% of gynostemma pentaphylla seed water extract, 10-15% of gynostemma pentaphylla seed fatty acid and 1.7-3.5% of a composite emulsifier are added;
(4) and (4) sequentially carrying out primary emulsification, homogenization treatment and freeze drying on the mixed solution obtained in the step (3) to obtain the gynostemma pentaphylla seed fatty acid microcapsule.
Further, the preparation method of the gynostemma pentaphylla seed aqueous extract in the step (1) specifically comprises the following steps:
101) preparing suspension from the powder of the gynostemma pentaphylla seeds left after the gynostemma pentaphylla seed oil is extracted;
102) ultrasonically treating the suspension in the step 101) for 20-40 min, standing for more than 12h under the condition of a water bath at the temperature of 35-45 ℃, and then centrifuging;
103) and (4) concentrating and drying the supernatant after the centrifugation treatment to obtain the gynostemma pentaphylla seed aqueous extract.
Further, the preparation steps of the gynostemma pentaphylla seed fatty acid in the step (2) specifically comprise:
201) adding 1mol/L sodium hydroxide solution into gynostemma pentaphylla seed oil to obtain saponification liquid, wherein the ratio of the gynostemma pentaphylla seed oil to the sodium hydroxide is 5 g: (0.1-0.2) mol, wherein the solvent in the sodium hydroxide solution is a mixture of distilled water and absolute ethyl alcohol in a volume ratio of 1: 9;
202) performing saponification reaction on the saponified solution obtained in the step 201) in a water bath at the temperature of 75-85 ℃ until the saponified solution is clear and transparent;
203) evaporating to remove ethanol in the clear and transparent saponified solution, adding 75-85 deg.C distilled water, adding hydrochloric acid to make the saponified solution delaminate, separating the upper layer, and washing with water to obtain the Gynostemma pentaphyllum seed fatty acid.
Further, the gynostemma pentaphylla seed oil is extracted from gynostemma pentaphylla seeds, and the extraction steps specifically comprise: firstly, smashing gynostemma pentaphylla seeds with the water content of less than 5% to 10-20 meshes, then placing the gynostemma pentaphylla seeds in a supercritical carbon dioxide extraction device, extracting for 120-150 min under the conditions that the extraction pressure is 25-40 MPa, the extraction temperature is 35-45 ℃, the separation pressure is 8-10 MPa, the separation temperature is 55-60 ℃ and the carbon dioxide flow rate is 20-30L/h, and finally separating to obtain the gynostemma pentaphylla seed oil.
Further, the compound emulsifier solution in the step (2) is formed by dissolving sucrose ester, monoglyceride and sodium alginate in water; in the mixed solution in the step (3), the sucrose ester accounts for 1-2% by mass, the monoglyceride accounts for 0.5-1% by mass, and the sodium alginate accounts for 0.2-0.5% by mass.
Further, in the step (4), primary emulsification is carried out under the shearing condition that the rotating speed is 8000-10000 r/min, and the shearing time is 3 minutes.
Further, the homogenization treatment in the step (4) is to homogenize for 2-4 times under 20-40 MPa.
Further, freezing for 8-16 h at-80 to-20 ℃ in the step (4).
A gynostemma pentaphylla seed fatty acid microcapsule prepared by the preparation method of the gynostemma pentaphylla seed fatty acid microcapsule is provided.
The application of the gynostemma pentaphylla seed fatty acid microcapsule in preparing anti-tumor and blood fat reducing medicines.
Compared with the prior art, the invention has the following beneficial technical effects:
the method takes gynostemma pentaphylla seed fatty acid as a core material, takes maltodextrin, soybean protein isolate and gynostemma pentaphylla seed water extract as wall materials, and prepares a powdery gynostemma pentaphylla seed fatty acid microcapsule product by emulsification and freeze drying technologies. The invention has simple preparation process, wide raw material source and low price. The edible protein and the aqueous extract of the gynostemma pentaphylla seeds are used as main wall materials, and the carbohydrate maltodextrin is added as a filling agent, so that the embedding rate of the microcapsule product exceeds 80%, the functional active ingredients of the fatty acid of the gynostemma pentaphylla seeds are greatly maintained while the oxygen is inhibited from entering, the oxidation stability of the gynostemma pentaphylla seeds is enhanced, and the shelf life is prolonged. According to a similar compatibility principle, the gynostemma pentaphylla seed water extract (GPWE) is added into the traditional wall material raw material to replace the function of soybean protein isolate, so that the embedding rate and the anti-tumor activity of the microcapsule are greatly improved while the biological activity of the core material is kept; the invention adopts a freeze-drying method, and the biological activity of the product is protected to the maximum extent; the microcapsule prepared by the invention has stable performance, is not easy to be oxidized, and has long shelf life and good biological activity.
Furthermore, sucrose ester and monoglyceride are used as composite emulsifiers, the hydrophilic-hydrophobic balance value is close to that of gynostemma pentaphylla seed fatty acid, and the emulsifying effect is good; sodium alginate is used as a stabilizer to increase the stability of an emulsification system.
The gynostemma pentaphylla seed fatty acid microcapsule product prepared by the method has uniform particle size, no cracks and depressions on the surface and good fluidity, and simultaneously improves the characteristic that fatty acid is insoluble in water.
[ description of the drawings ]
FIG. 1 is a flow chart of the present invention.
Fig. 2(a) and 2(b) are graphs showing the effect of microcapsules of example 1 on the survival of K562 cells and CT26 cells.
Fig. 3(a) and 3(b) are graphs showing the effect of microcapsules in comparative example 1 on the survival of K562 cells and CT26 cells.
FIGS. 4(a) to 4(d) are graphs showing the effects of the microcapsules of example 1 and comparative example 2 on four blood lipids in diabetic mice.
[ detailed description ] embodiments
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The technical scheme of the invention is as follows: taking gynostemma pentaphylla seed fatty acid (GPFA) as a core material, taking maltodextrin, soybean protein isolate and gynostemma pentaphylla seed water extract (GPWE) as wall materials, taking sucrose ester and monoglyceride as composite emulsifiers, taking sodium alginate as an antioxidant, and preparing a powdery GPFA microcapsule product by a freeze-drying technology.
The preparation method comprises the steps of preparation of Gynostemma Pentaphylla Seed Oil (GPSO), extraction of GPWE, preparation of a wall material phase, blending of an emulsifier, preparation of a core material phase, mixing, primary emulsification, homogenization, freeze drying and the like. Referring to fig. 1, the method comprises the following specific steps:
(1) preparation of gynostemma pentaphylla seed oil (g. pentaphylum seed oil, GPSO): the method comprises the steps of crushing gynostemma pentaphylla seeds with the water content of less than 5% to 10-20 meshes, placing the gynostemma pentaphylla seeds in a supercritical carbon dioxide extraction device, setting the extraction pressure to be 25-40 MPa, the extraction temperature to be 35-45 ℃, the separation pressure to be 8-10 MPa and the separation temperature to be 55-60 ℃, controlling the flow rate of carbon dioxide to be 20-30L/h, extracting for 120-150 min, and collecting separation products to obtain gynostemma pentaphylla seed oil.
(2) Preparation of gynostemma pentaphylla seed fatty acid (GPFA): weighing 5g of gynostemma pentaphylla seed oil in a 250mL round-bottom flask, adding 100-200 mL of 1mol/L sodium hydroxide solution, and connecting with a condensation reflux device; wherein the solvent in the sodium hydroxide solution is a mixture of distilled water and absolute ethyl alcohol in a volume ratio of 1:9, and the ratio of the gynostemma pentaphylla seed oil to the sodium hydroxide is 5 g: (0.1-0.2) mol. Heating and saponifying in water bath at 75-85 deg.c for 1-2 hr to react oil and fat completely until the saponified liquid is clear and transparent. Then, removing ethanol by rotary evaporation, adding hot distilled water at 75-85 ℃ to dissolve reaction products, and ensuring that no obvious solid exists in saponification liquid; and (3) adding dilute hydrochloric acid into the alkaline saponification solution, continuously shaking the flask, finding that the saponification solution is layered, wherein the upper layer is fatty acid, the lower layer is acidic glycerol solution, adjusting the pH value of the lower layer to 1.5-2, separating the upper layer of fatty acid, washing the upper layer of fatty acid with hot distilled water, washing for several times until the water phase of the lower layer is neutral, and collecting the upper layer of fatty acid to obtain the gynostemma pentaphylla seed fatty acid.
(3) Preparation of an aqueous extract of gynostemma pentaphyllum seeds (The water extract of g. pentaphylum seeds, GPWE): sieving the powder remaining after the oil extraction of the gynostemma pentaphylla seeds by a sieve of 70-90 meshes, weighing 100g of the powder, dissolving the powder in 1L of distilled water, and preparing into suspension with the concentration of 0.1 kg/L; and (3) carrying out ultrasonic treatment on the suspension for 20-40 min, standing in a water bath at the temperature of 35-45 ℃ for more than 12h, centrifuging for 10min at the speed of 8000-10000 r/min, concentrating the supernatant by using a rotary evaporator, and drying the concentrated solution by using a freeze dryer to obtain an aqueous extract of gynostemma pentaphylla seed powder, wherein the main components of the aqueous extract are protein and a small amount of polysaccharide.
(4) Preparation of wall material phase: weighing maltodextrin, soy protein isolate and GPWE in water, and mixing uniformly to form a wall material phase solution.
(5) Blending of an emulsifier: weighing sucrose ester, monoglyceride and sodium alginate, dissolving in water, and mixing to obtain compound emulsifier solution.
(6) Preparation of core material phase: and (3) weighing the GPFA obtained in the step (2), and adding the GPFA into the composite emulsifier solution formed in the step (5) to form a core phase solution.
(7) Mixing: mixing the wall material phase solution and the core material phase solution according to a ratio of 2:1, and uniformly stirring to obtain a mixed solution; the mass of the mixed solution is A, the mass of maltodextrin is 10-15% A, the mass fraction of the soybean protein isolate is 5-10% A, the mass fraction of GPWE is 5-10% A, and the mass fraction of GPFA is 10-15% A; the mass fraction of sucrose ester is 1-2% A, the mass fraction of monoglyceride is 0.5-1% A, and the mass fraction of sodium alginate is 0.2-0.5% A;
(8) primary emulsification: carrying out primary emulsification on the mixed solution obtained in the step (7) through high-shear emulsification, wherein the shearing rotating speed is 8000-10000 r/min, and the shearing time is 3 min;
(9) homogenizing: homogenizing the microcapsule emulsion obtained in the step (8) for 2-4 times under high pressure of 20-40 MPa to form O/W (oil/water) emulsion;
(10) and (3) freeze drying: and (3) filling the O/W (oil/water) emulsion obtained in the step (9) into a glass culture dish (phi =15 cm), freezing in a freeze dryer, freezing at-80 to-20 ℃ for 8-16 h, and taking out to obtain a microcapsule product. The thickness of the emulsion is not more than 5mm, because the thickness is too large, water residue is easy to exist, and the freezing time is prolonged;
unless otherwise specified,% in the present invention means mass fraction in terms of W/W.
For better understanding of the present invention, the following examples are given to illustrate the present invention in further detail, but the present invention is not limited to the following examples.
Example 1:
a preparation process of gynostemma pentaphylla seed fatty acid microcapsules comprises the following steps:
(1) preparation of gynostemma pentaphylla seed oil (g. pentaphylum seed oil, GPSO): pulverizing Gynostemma pentaphyllum Makino seeds with water content less than 5% to 10 mesh, placing in a supercritical carbon dioxide extraction device, extracting at 20L/h under the conditions of extraction pressure of 25MPa, extraction temperature of 35 deg.C, separation pressure of 8MPa and separation temperature of 55 deg.C for 120min, and collecting the separated product to obtain Gynostemma pentaphyllum Makino seed oil.
(2) Preparation of gynostemma pentaphylla seed fatty acid (GPFA): weighing 5g of gynostemma pentaphylla seed oil in a 250mL round-bottom flask, adding 100mL of 1mol/L sodium hydroxide ethanol solution, and connecting with a condensing reflux device. Heating in 75 deg.C water bath for about 1 hr for saponification to allow oil to react completely, and saponifying the solution until it is clear and transparent. Then rotary evaporating to remove ethanol, adding hot distilled water (75 deg.C) to dissolve, adding dilute hydrochloric acid, shaking flask continuously to find saponification solution layer by layer, upper layer is fatty acid, lower layer is acidic glycerol solution, adjusting lower layer pH to 1.5-2, separating upper layer fatty acid, washing upper layer fatty acid with hot distilled water, washing several times, and collecting upper layer until lower layer water phase is neutral to obtain herba Gynostemmatis seed fatty acid.
(3) Preparation of an aqueous extract of gynostemma pentaphyllum seeds (The water extract of g. pentaphylum seeds, GPWE): sieving the powder left after oil extraction of the gynostemma pentaphylla seeds with a 80-mesh sieve, weighing 100g of the powder, dissolving the powder in 1L of distilled water, carrying out ultrasonic treatment for 30min, standing the solution in a water bath at 35 ℃ for 12h, centrifuging the solution at 8000r/min for 10min, taking the supernatant, concentrating the supernatant by using a rotary evaporator, and drying the concentrated solution by using a freeze dryer to obtain an aqueous extract of the gynostemma pentaphylla seeds, wherein the main component is protein. There are also some polysaccharide components.
(4) Preparation of wall material phase: weighing maltodextrin, soy protein isolate and GPWE in water, and mixing uniformly to form a wall material phase solution.
(5) Blending of an emulsifier: weighing sucrose ester, monoglyceride and sodium alginate, dissolving in water, and mixing to obtain compound emulsifier solution.
(6) Preparation of core material phase: and (3) weighing the GPFA obtained in the step (2), and adding the GPFA into the composite emulsifier solution formed in the step (5) to form a core phase solution.
(7) Mixing: mixing the wall material phase solution and the core material phase solution according to a ratio of 2:1, and uniformly stirring to obtain a mixed solution; the mass of the mixed solution is A, the mass of the maltodextrin is 10% A, the mass fraction of the soybean protein isolate is 5% A, the mass fraction of the GPWE is 10% A, and the mass fraction of the GPFA is 10% A; the mass fraction of sucrose ester is 1% A, the mass fraction of monoglyceride is 0.5% A, and the mass fraction of sodium alginate is 0.2% A;
(8) primary emulsification: carrying out primary emulsification on the mixed solution obtained in the step (7) through high shear emulsification, wherein the shear rotation speed is 8000r/min, and the shear time is 3 min;
(9) homogenizing: homogenizing the microcapsule emulsion obtained in the step (8) for 2 times under high pressure of 20MPa to form O/W (oil/water) emulsion;
(10) and (3) freeze drying: and (3) filling the O/W (oil/water) emulsion obtained in the step (9) into a glass culture dish (phi =15 cm), freezing in a freeze dryer, freezing at-80 ℃ for 16h, and taking out to obtain a microcapsule product. The thickness of the emulsion is not more than 5mm, because the thickness is too large, water residue is easy to exist, and the freezing time is prolonged;
example 2:
a preparation process of gynostemma pentaphylla seed fatty acid microcapsules comprises the following steps:
(1) preparation of gynostemma pentaphylla seed oil (g. pentaphylum seed oil, GPSO): pulverizing Gynostemma pentaphyllum Makino seeds with water content less than 5% to 10 mesh, placing in a supercritical carbon dioxide extraction device, setting extraction pressure at 40MPa, extraction temperature at 45 deg.C, separation pressure at 10MPa, separation temperature at 60 deg.C, controlling carbon dioxide flow rate at 30L/h, extracting for 150min, and collecting separated product to obtain Gynostemma pentaphyllum Makino seed oil.
(2) Preparation of gynostemma pentaphylla seed fatty acid (GPFA): weighing 5g of gynostemma pentaphylla seed oil in a 250mL round-bottom flask, adding 200mL of 1mol/L sodium hydroxide-90% ethanol solution, and connecting with a condensing reflux device. Heating in water bath at 85 deg.C for about 2 hr for reacting oil and fat, and saponifying until clear and transparent. Then rotary evaporating to remove ethanol, adding hot distilled water (85 deg.C) to dissolve, adding dilute hydrochloric acid, shaking flask continuously to find saponification solution layer by layer, upper layer is fatty acid, lower layer is acidic glycerol solution, adjusting lower layer pH to 1.5-2, separating upper layer fatty acid, washing upper layer fatty acid with hot distilled water, washing several times, and collecting upper layer until lower layer water phase is neutral to obtain herba Gynostemmatis seed fatty acid.
(3) Preparation of an aqueous extract of gynostemma pentaphyllum seeds (The water extract of g. pentaphylum seeds, GPWE): sieving the powder remained after the oil extraction of the gynostemma pentaphylla seeds with a 80-mesh sieve, weighing 100g of the powder, dissolving the powder in 1L of distilled water, carrying out ultrasonic treatment for 30min, standing the solution in a water bath at 40 ℃ for 15h, centrifuging the solution at 10000r/min for 10min, taking the supernatant, concentrating the supernatant by using a rotary evaporator, and drying the concentrated solution by using a freeze dryer to obtain an aqueous extract of the gynostemma pentaphylla seeds, wherein the main component is protein. There are also some polysaccharide components.
(4) Preparation of wall material phase: weighing maltodextrin, soy protein isolate and GPWE in water, and mixing uniformly to form a wall material phase solution.
(5) Blending of an emulsifier: weighing sucrose ester, monoglyceride and sodium alginate, dissolving in water, and mixing to obtain compound emulsifier solution.
(6) Preparation of core material phase: and (3) weighing the GPFA obtained in the step (2), and adding the GPFA into the composite emulsifier solution formed in the step (5) to form a core phase solution.
(7) Mixing: mixing the wall material phase solution and the core material phase solution according to a ratio of 2:1, and uniformly stirring to obtain a mixed solution; the mass of the mixed solution is A, the mass of the maltodextrin is 15% A, the mass fraction of the soybean protein isolate is 10% A, the mass fraction of the GPWE is 5% A, and the mass fraction of the GPFA is 15% A; wherein the mass fraction of the sucrose ester is 2% A, the mass fraction of the monoglyceride is 1% A, and the mass fraction of the sodium alginate is 0.5% A.
(8) Primary emulsification: carrying out primary emulsification on the mixed solution obtained in the step (7) through high shear emulsification, wherein the shear rotation speed is 10000r/min, and the shear time is 3 min;
(9) homogenizing: homogenizing the microcapsule emulsion obtained in the step (8) for 4 times under high pressure of 40MPa to form O/W (oil/water) emulsion;
(10) and (3) freeze drying: and (3) filling the O/W (oil/water) emulsion obtained in the step (9) into a glass culture dish (phi =15 cm), freezing in a freeze dryer, freezing at-80 ℃ for 12h, and taking out to obtain a microcapsule product. The thickness of the emulsion is not more than 5mm, because the thickness is too large, water residue is easy to exist, and the freezing time is prolonged;
example 3
A preparation process of gynostemma pentaphylla seed fatty acid microcapsules comprises the following steps:
(1) preparation of gynostemma pentaphylla seed oil (g. pentaphylum seed oil, GPSO): pulverizing Gynostemma pentaphyllum Makino seeds with water content less than 5% to 15 meshes, placing in a supercritical carbon dioxide extraction device, setting extraction pressure at 35MPa, extraction temperature at 40 deg.C, separation pressure at 9MPa, separation temperature at 57 deg.C, controlling carbon dioxide flow rate at 25L/h, extracting for 135min, and collecting separated product to obtain Gynostemma pentaphyllum Makino seed oil.
(2) Preparation of gynostemma pentaphylla seed fatty acid (GPFA): weighing 5g of gynostemma pentaphylla seed oil in a 250mL round-bottom flask, adding 150mL of 1mol/L sodium hydroxide-90% ethanol solution, and connecting with a condensing reflux device. Heating in 80 deg.C water bath for saponification for about 1.5 hr to allow oil to react sufficiently, and saponifying the solution until it is clear and transparent. Then rotary evaporating to remove ethanol, adding hot distilled water (80 deg.C) to dissolve, adding dilute hydrochloric acid, shaking the flask, separating upper fatty acid layer when the saponification solution is layered, the upper fatty acid layer is fatty acid and the lower acidic glycerol layer is acidic, adjusting the pH value of the lower fatty acid layer to 1.5-2, washing the upper fatty acid layer with hot distilled water, washing several times, and collecting the upper fatty acid layer when the water phase of the lower fatty acid layer is neutral.
(3) Preparation of an aqueous extract of gynostemma pentaphyllum seeds (The water extract of g. pentaphylum seeds, GPWE): sieving the powder left after oil extraction of the gynostemma pentaphylla seeds with a 80-mesh sieve, weighing 100g of the powder, dissolving the powder in 1L of distilled water, carrying out ultrasonic treatment for 30min, standing the solution in a water bath at 45 ℃ for 14h, centrifuging the solution at 9000r/min for 10min, taking the supernatant, concentrating the supernatant by using a rotary evaporator, and drying the concentrated solution by using a freeze dryer to obtain an aqueous extract of the gynostemma pentaphylla seed powder, wherein the main component is protein. There are also some polysaccharide components.
(4) Preparation of wall material phase: weighing maltodextrin, soy protein isolate and GPWE in water, and mixing uniformly to form a wall material phase solution.
(5) Blending of an emulsifier: weighing sucrose ester, monoglyceride and sodium alginate, dissolving in water, and mixing to obtain compound emulsifier solution.
(6) Preparation of core material phase: and (3) weighing the GPFA obtained in the step (2), and adding the GPFA into the composite emulsifier solution formed in the step (3) to form a core phase solution.
(7) Mixing: mixing the wall material phase solution and the core material phase solution according to a ratio of 2:1, and uniformly stirring to obtain a mixed solution; the mass of the mixed solution is A, the mass of the maltodextrin is 12% A, the mass fraction of the soybean protein isolate is 7% A, the mass fraction of the GPWE is 8% A, and the mass fraction of the GPFA is 12% A; wherein the mass fraction of sucrose ester is 1.5% A, the mass fraction of monoglyceride is 0.7% A, and the mass fraction of sodium alginate is 0.35% A.
(9) Primary emulsification: carrying out primary emulsification on the mixed solution obtained in the step (5) through high-shear emulsification, wherein the shearing rotating speed is 9000r/min, and the shearing time is 3 minutes;
(10) homogenizing: homogenizing the microcapsule emulsion obtained in the step (6) for 3 times under the high pressure of 30MPa to form O/W (oil/water) emulsion;
(11) and (3) freeze drying: and (3) filling the O/W (oil/water) emulsion obtained in the step (10) into a glass culture dish (phi =15 cm), freezing in a freeze dryer, freezing at-20 ℃ for 8h, and taking out to obtain a microcapsule product. The thickness of the emulsion is not more than 5mm, because the thickness is too large, water residue is easy to exist, and the freezing time is prolonged;
the method comprises the steps of preparation of gynostemma pentaphylla seed oil, preparation of self-fatty acid in gynostemma pentaphylla, preparation of gynostemma pentaphylla seed water-soluble protein, preparation of wall material phase, blending of emulsifier, preparation of core material phase, mixing, primary emulsification, homogenization, freeze drying and the like. Greatly maintains the functional active ingredients of the gynostemma pentaphylla seed fatty acid, enhances the oxidation stability of the gynostemma pentaphylla seed fatty acid, covers the bad smell of the gynostemma pentaphylla seed fatty acid and improves the product quality. Meanwhile, the method converts the gynostemma pentaphylla seed fatty acid from liquid state to stable solid state form, is convenient for storage and transportation, is beneficial to the occurrence of the gynostemma pentaphylla seed fatty acid in a multi-form product mode, enlarges the application range of the gynostemma pentaphylla seed fatty acid, and meets the diversified requirements of consumers.
The microcapsule of the invention is redissolved after freeze drying, has good solubility, can stably exist for 30 days, and has the particle size range of 2-3 microns.
The microcapsule prepared by the invention has a certain killing effect on tumor cells and also has a certain effect on insulin resistance.
Comparative example 1: without addition of GPWE
(1) Preparation of gynostemma pentaphylla seed oil (g. pentaphylum seed oil, GPSO): pulverizing Gynostemma pentaphyllum Makino seeds with water content less than 5% to 15 meshes, placing in a supercritical carbon dioxide extraction device, setting extraction pressure at 35MPa, extraction temperature at 40 deg.C, separation pressure at 9MPa, separation temperature at 55 deg.C, controlling carbon dioxide flow rate at 25L/h, extracting for 135min, and collecting separated product to obtain Gynostemma pentaphyllum Makino seed oil.
(2) Preparation of gynostemma pentaphylla seed fatty acid (GPFA): weighing 5g of gynostemma pentaphylla seed oil in a 250mL round-bottom flask, adding 100mL of 1mol/L sodium hydroxide-90% ethanol solution, and connecting with a condensing reflux device. Heating in 80 deg.C water bath for saponification for about 1 hr to allow oil to react sufficiently, and saponifying the solution until it is clear and transparent. Then rotary evaporating to remove ethanol, adding hot distilled water (80 deg.C) to dissolve, adding dilute hydrochloric acid, shaking the flask, separating upper fatty acid layer when the saponification solution is layered, the upper fatty acid layer is fatty acid and the lower acidic glycerol layer is acidic, adjusting the pH value of the lower fatty acid layer to 1.5-2, washing the upper fatty acid layer with hot distilled water, washing several times, and collecting the upper fatty acid layer when the water phase of the lower fatty acid layer is neutral.
(3) Preparation of wall material phase: weighing maltodextrin and soybean protein isolate in water and mixing uniformly to form a wall material phase solution.
(4) Blending of an emulsifier: weighing sucrose ester, monoglyceride and sodium alginate, dissolving in water, and mixing to obtain compound emulsifier solution.
(6) Preparation of core material phase: and (3) weighing the GPFA obtained in the step (2), and adding the GPFA into the composite emulsifier solution formed in the step (5) to form a core phase solution.
(7) Mixing: mixing the wall material phase solution and the core material phase solution according to a ratio of 2:1, and uniformly stirring to obtain a mixed solution; the mass of the mixed solution is A, the mass of the maltodextrin is 10% A, the mass fraction of the soybean protein isolate is 15% A, and the mass of the GPFA is 10% A; wherein the mass fraction of sucrose ester is 1% A, the mass fraction of monoglyceride is 0.5% A, and the mass fraction of sodium alginate is 0.2% A.
(8) Primary emulsification: carrying out primary emulsification on the mixed solution obtained in the step (7) through high shear emulsification, wherein the shear rotation speed is 8000r/min, and the shear time is 3 min;
(9) homogenizing: homogenizing the microcapsule emulsion obtained in the step (6) for 4 times under high pressure of 40MPa to form O/W (oil/water) emulsion;
(10) and (3) freeze drying: and (3) filling the O/W (oil/water) emulsion obtained in the step (10) into a glass culture dish (phi =15 cm), freezing in a freeze dryer, freezing at-80 ℃ for 12h, and taking out to obtain a microcapsule product. The thickness of the emulsion is not more than 5mm, because the thickness is too large, water residue is easy to exist, and the freezing time is prolonged;
comparative example 2: without addition of GPFA
(1) Preparation of gynostemma pentaphylla seed oil (g. pentaphylum seed oil, GPSO): pulverizing Gynostemma pentaphyllum Makino seeds with water content less than 5% to 15 meshes, placing in a supercritical carbon dioxide extraction device, setting extraction pressure at 35MPa, extraction temperature at 40 ℃, separation pressure at 9MPa, separation temperature at 55 ℃, controlling carbon dioxide flow rate at 25L/h, extracting for 13min, and collecting separation products to obtain Gynostemma pentaphyllum Makino seed oil.
(2) Preparation of an aqueous extract of gynostemma pentaphyllum seeds (The water extract of g. pentaphylum seeds, GPWE): sieving the powder remained after the oil extraction of the gynostemma pentaphylla seeds with a 80-mesh sieve, weighing 100g of the powder, dissolving the powder in 1L of distilled water, carrying out ultrasonic treatment for 30min, carrying out water bath at 40 ℃ overnight, centrifuging the powder at 10000r/min for 10min, taking the supernatant, concentrating the supernatant by using a rotary evaporator, and drying the concentrated solution by using a freeze dryer to obtain the gynostemma pentaphylla seed powder water extract, wherein the main component is protein. There are also some polysaccharide components.
(3) Preparation of wall material phase: weighing maltodextrin, soy protein isolate and GPWE in water, and mixing uniformly to form a wall material phase solution.
(4) Blending of an emulsifier: weighing sucrose ester, monoglyceride and sodium alginate, dissolving in water, and mixing to obtain compound emulsifier solution.
(5) Mixing: mixing the wall material phase solution with an emulsifier according to a ratio of 2:1, and uniformly stirring to obtain a mixed solution; the mass of the mixed solution is A, the mass of maltodextrin is 10% A, the mass fraction of the isolated soy protein is 10% A, the mass fraction of GPWE is 5% A, wherein the mass fraction of sucrose ester is 1% A, the mass fraction of monoglyceride is 0.5% A, and the mass fraction of sodium alginate is 0.2% A.
(6) Primary emulsification: carrying out primary emulsification on the mixed solution obtained in the step (5) through high shear emulsification, wherein the shear rotation speed is 10000r/min, and the shear time is 3 min;
(7) homogenizing: homogenizing the microcapsule emulsion obtained in the step (6) for 4 times under high pressure of 40MPa to form O/W (oil/water) emulsion;
(8) and (3) freeze drying: and (3) filling the O/W (oil/water) emulsion obtained in the step (10) into a glass culture dish (phi =15 cm), freezing in a freeze dryer, freezing at-80 ℃ for 12h, and taking out to obtain a microcapsule product.
The thickness of the emulsion is not more than 5mm, because the thickness is too large and moisture residue is easy to occur, and the freezing time is required to be prolonged.
The experimental steps are as follows: both K562 and CT26 were cultured in RPIM1640 complete medium (10% fetal bovine serum + 1% glutamine + 1% diabody (streptomycin and penicillin) in incubator (5% carbon dioxide at 37 ℃ C.) CT26 was digested with 0.05% trypsin when the cells grew to logarithmic growth phase, counted, and cell density was adjusted to 1X 105seed/mL, inoculationCells were grown in 96-well plates to the point where K562 cells grew to log phase. Setting 6 multiple wells for each concentration, adding medicine after each 100 mu l of cell is attached to the wall for 12-14h, adding 20 mu l of MTT (3- (4, 5-dimethylthiazole-2) -2, 5-diphenyl tetrazole bromide) into each well after culturing for 24 h, removing the culture solution after 4h, adding 150 mu l of dimethyl sulfoxide, directly adding a triple solution (weighing 10g of dodecyl sulfate to be dissolved in 95mL of triple distilled water, adding 5mL of isobutanol and 0.1mL of concentrated hydrochloric acid, uniformly mixing, filtering and sterilizing a 0.22 mu m filter membrane, storing in a dark place) for 150r 15min, and detecting and absorbing at 570nm, wherein the culture solution is removed after K562 is not required to remove the culture medium.
From fig. 2(a), fig. 2(b), fig. 3(a) and fig. 3 (b): as can be seen from the comparison between fig. 2(a) and fig. 3(a), compared with the microcapsule product without GPWE added in the wall material, the addition of GPWE can significantly enhance the killing effect of the product on K562 cells; the same effect is shown in fig. 2(b) and 3 (b). Therefore, the invention can be used for developing anti-tumor drugs.
In FIGS. 4(a) to 4(d), # # denotes P < 0.01# P < 0.05, compared to the control group; p < 0.01 × P < 0.05 relative to model group.
Establishing a diabetes model: kunming mice (18-22g) purchased from fourth Leguminosae medical university are adaptively fed for one week, fed for one month at high fat, injected with 40mg/kg of streptozotocin, injected once every three days for 3 times, and the fasting blood glucose is measured on the second day, the modeling success is realized by taking the blood glucose concentration of more than 7.8mmol/L, otherwise, the injection is performed once every other day. High fat feeding is continued for one month, group treatment is carried out for one month, and a control group and a model group are fed with physiological saline. One month later, mice were sacrificed to detect four blood lipids and other related indicators.
As can be seen from fig. 4(a) to 4(d), the microcapsule containing gynostemma pentaphylla seed fatty acid can significantly reduce TC, TG and LDL in serum, and simultaneously can increase HDL in serum, and has a certain protective effect on diabetic mice.
In conclusion, the gynostemma pentaphylla seed fatty acid microcapsule has the effects of resisting tumors and reducing blood fat, and compared with western medicines, the traditional Chinese medicine is safe and has few side effects; no damage to gastrointestinal tract; has the advantages of little damage to liver and kidney, etc. Can replace western medicines, reduce the dosage of the western medicines, and reduce the toxicity of liver and kidney, and can be used for developing functional health products for reducing blood lipid.
Claims (8)
1. A preparation method of gynostemma pentaphylla seed fatty acid microcapsules is characterized by comprising the following steps: the method comprises the following steps:
(1) dissolving maltodextrin, soy protein isolate and gynostemma pentaphylla seed aqueous extract in water, and uniformly mixing to form a wall material phase solution;
(2) adding the gynostemma pentaphylla seed fatty acid into the composite emulsifier solution to form a core material phase solution;
(3) mixing the wall material phase solution and the core material phase solution, and uniformly stirring to obtain a mixed solution; in the mixed solution, by mass percent, 10-15% of maltodextrin, 5-10% of soybean protein isolate, 5-10% of gynostemma pentaphylla seed water extract, 10-15% of gynostemma pentaphylla seed fatty acid and 1.7-3.5% of a composite emulsifier are added;
(4) sequentially carrying out primary emulsification, homogenization treatment and freeze drying on the mixed solution obtained in the step (3) to obtain gynostemma pentaphylla seed fatty acid microcapsules;
the preparation method of the gynostemma pentaphylla seed aqueous extract in the step (1) specifically comprises the following steps:
101) preparing suspension from the powder of the gynostemma pentaphylla seeds left after the gynostemma pentaphylla seed oil is extracted;
102) ultrasonically treating the suspension in the step 101) for 20-40 min, standing for more than 12h under the condition of a water bath at the temperature of 35-45 ℃, and then centrifuging;
103) concentrating and drying the supernatant after the centrifugation treatment to obtain a gynostemma pentaphylla seed water extract;
the preparation method of the gynostemma pentaphylla seed fatty acid in the step (2) specifically comprises the following steps:
201) adding 1mol/L sodium hydroxide solution into gynostemma pentaphylla seed oil to obtain saponification liquid, wherein the ratio of the gynostemma pentaphylla seed oil to the sodium hydroxide is 5 g: (0.1-0.2) mol, wherein the solvent in the sodium hydroxide solution is a mixture of distilled water and absolute ethyl alcohol in a volume ratio of 1: 9;
202) performing saponification reaction on the saponified solution obtained in the step 201) in a water bath at the temperature of 75-85 ℃ until the saponified solution is clear and transparent;
203) evaporating to remove ethanol in the clear and transparent saponified solution, adding 75-85 deg.C distilled water, adding hydrochloric acid to make the saponified solution delaminate, separating the upper layer, and washing with water to obtain the Gynostemma pentaphyllum seed fatty acid.
2. The preparation method of gynostemma pentaphylla seed fatty acid microcapsule according to claim 1, wherein the step of preparing the gynostemma pentaphylla seed fatty acid microcapsule comprises the following steps: the gynostemma pentaphylla seed oil is extracted from gynostemma pentaphylla seeds, and the extraction steps specifically comprise: firstly, smashing gynostemma pentaphylla seeds with the water content of less than 5% to 10-20 meshes, then placing the gynostemma pentaphylla seeds in a supercritical carbon dioxide extraction device, extracting for 120-150 min under the conditions that the extraction pressure is 25-40 MPa, the extraction temperature is 35-45 ℃, the separation pressure is 8-10 MPa, the separation temperature is 55-60 ℃ and the carbon dioxide flow rate is 20-30L/h, and finally separating to obtain the gynostemma pentaphylla seed oil.
3. The preparation method of gynostemma pentaphylla seed fatty acid microcapsule according to claim 1, wherein the step of preparing the gynostemma pentaphylla seed fatty acid microcapsule comprises the following steps: the compound emulsifier solution in the step (2) is formed by dissolving sucrose ester, monoglyceride and sodium alginate in water; in the mixed solution in the step (3), the sucrose ester accounts for 1-2% by mass, the monoglyceride accounts for 0.5-1% by mass, and the sodium alginate accounts for 0.2-0.5% by mass.
4. The preparation method of gynostemma pentaphylla seed fatty acid microcapsule according to claim 1, wherein the step of preparing the gynostemma pentaphylla seed fatty acid microcapsule comprises the following steps: in the step (4), primary emulsification is carried out under the shearing condition that the rotating speed is 8000-10000 r/min, and the shearing time is 3 minutes.
5. The preparation method of gynostemma pentaphylla seed fatty acid microcapsule according to claim 1, wherein the step of preparing the gynostemma pentaphylla seed fatty acid microcapsule comprises the following steps: the homogenization treatment in the step (4) is to homogenize for 2-4 times under 20-40 MPa.
6. The preparation method of gynostemma pentaphylla seed fatty acid microcapsule according to claim 1, wherein the step of preparing the gynostemma pentaphylla seed fatty acid microcapsule comprises the following steps: freezing for 8-16 h at-80-20 ℃ in the step (4).
7. A gynostemma pentaphylla seed fatty acid microcapsule prepared by the preparation method of the gynostemma pentaphylla seed fatty acid microcapsule of claim 1.
8. The application of the gynostemma pentaphylla seed fatty acid microcapsule in preparing anti-tumor and blood fat reducing medicines according to claim 7.
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