Nauclea officinalis extract capsule and production process thereof

Abstract

The invention discloses a nauclea officinalis extract capsule and a production process thereof, and belongs to the technical field of capsules, the production process comprises the following steps: crushing nauclea officinalis, sieving, then adding an ethanol water solution, uniformly mixing with an extraction auxiliary material, heating, extracting, filtering, repeatedly extracting for 2-4 times, combining filtrate, and concentrating under reduced pressure to obtain nauclea officinalis extract; performing spray drying on the nauclea officinalis extract to obtain nauclea officinalis extract powder; adding the microcapsule wall material compound into water, stirring, then adding nauclea officinalis extract powder, uniformly mixing, homogenizing under high pressure, concentrating under reduced pressure after the homogenizing is finished, and then performing spray drying to obtain nauclea officinalis extract microcapsules; uniformly mixing the nauclea officinalis extract microcapsules, corn starch and microcrystalline cellulose, granulating, drying, finishing granules, adding magnesium stearate, uniformly mixing, and filling into hollow capsules to obtain the nauclea officinalis extract capsules. The nauclea officinalis extract capsule produced by the invention has good effects of clearing away heat and toxic materials, diminishing inflammation and relieving pain, and is high in bioavailability and stable in effect.

Description

Technical Field

[0001] The invention relates to the technical field of capsules, and in particular to a gallwood extract capsule and a production process thereof. Background Art

[0002] Gallwood, also known as black sandalwood, bear gall tree, yellow heart wood, tree yellow cork, etc., is mainly distributed in Guangdong, Guangxi, Hainan and other regions. It is the dried branches (with skin) of the black sandalwood plant of the Rubiaceae family. Gallwood has good heat-clearing, detoxifying and anti-inflammatory effects, and is suitable for the treatment of a variety of diseases, including colds and fevers, sore throats, external auditory canal furuncles, skin furuncles, acute conjunctivitis, acute jaundice, stomachache, etc. Gallwood extract is a high-concentration extract concentrated from the active ingredients extracted from gallwood through modern extraction technology and processes, mainly including alkaloids, flavonoids, phenolic compounds, etc. Gallwood extract has an inhibitory effect on a variety of bacteria and can be used to treat infectious diseases caused by bacteria; it can reduce inflammatory reactions and is suitable for the treatment of various inflammatory diseases. Gallwood extract is widely used in the production of traditional Chinese medicine preparations due to its high efficiency and safety. It can process and produce a variety of traditional Chinese medicine preparations, such as granules, tablets, capsules, oral liquids, etc., to meet different usage needs. Among them, the Gallwood Extract Capsule is a traditional Chinese medicine preparation that encapsulates Gallwood Extract in a capsule shell. The capsule form is convenient for patients to take and can prevent it from being affected by moisture, oxidation and other problems.

[0003] Chinese patent CN111000914A discloses a sustained-release capsule of gallwood extract and a preparation method thereof, wherein the sustained-release capsule comprises a hollow capsule and a quick-release pill, a medium-release pill and a slow-release pill filled in the hollow capsule; wherein the quick-release pill comprises 120-140 parts of gallwood extract powder, 60-80 parts of dextrin and 7-9 parts of magnesium stearate; the medium-release pill comprises 120-140 parts of gallwood extract powder, 30-50 parts of hydroxypropyl methylcellulose, 4-6 parts of polyvinyl pyrrolidone, 60-80 parts of dextrin and 7-9 parts of magnesium stearate. 9 parts; the slow pills include 120-140 parts of gallwood extract powder, 60-100 parts of hydroxypropyl methylcellulose, 8-12 parts of polyvinyl pyrrolidone, 60-80 parts of dextrin and 7-9 parts of magnesium stearate; the gallwood extract capsules prepared by the patent can continuously release drugs, have a long drug release time, and can be slowly released in the body, thereby making the blood drug concentration in the body more stable; however, the preparation process of the above-mentioned gallwood extract sustained-release capsules is relatively cumbersome, and the biological activity of the gallwood extract is greatly lost, and the problem of poor efficacy stability will also occur during storage. Summary of the invention

[0004] In view of the deficiencies in the above-mentioned prior art, the present invention provides a gallwood extract capsule, which further improves the biological activity of the gallwood extract by optimizing the extraction steps and simultaneously microencapsulating the gallwood extract, so that it has better heat-clearing and detoxifying and anti-inflammatory and analgesic effects, and the gallwood extract microcapsule has stable efficacy and high bioavailability. The present invention also provides a production process for the gallwood extract capsule.

[0005] The technical solution adopted by the present invention is:

[0006] The present invention provides a production process of gallwood extract capsules, comprising the following steps:

[0007] Step I: crush the gallwood and sieve it, then add ethanol water solution and extraction auxiliary materials to mix evenly, heat extraction, filter, repeat extraction 2-4 times, combine the filtrate, and concentrate under reduced pressure to obtain gallwood extract; spray dry the gallwood extract to obtain gallwood extract powder;

[0008] Step II: adding the microcapsule wall material composite into water and stirring, then adding the gallwood extract powder and mixing evenly, high pressure homogenization, and then concentrating under reduced pressure, and then spray drying to obtain gallwood extract microcapsules;

[0009] Step III: uniformly mix the gallwood extract microcapsules, corn starch and microcrystalline cellulose, granulate, dry, and granulate, add magnesium stearate and mix evenly, and then fill into hollow capsules to obtain the gallwood extract capsules.

[0010] Preferably, a production process of gallwood extract capsules comprises the following steps:

[0011] Step I: crush the gallwood and pass it through an 80-150 mesh sieve, then add 75-78wt% ethanol aqueous solution and extraction auxiliary materials and mix them evenly, extract at 80-85°C for 80-100 minutes, filter, repeat the extraction 2-4 times, combine the obtained filtrate, and reduce the pressure to concentrate the filtrate to 8-12% of the original weight to obtain gallwood extract; spray dry the gallwood extract to obtain gallwood extract powder;

[0012] Step II: adding 2-4 parts by weight of the microcapsule wall material composite to 180-220 parts by weight of water, stirring at 200-500 r / min for 10-30 min, then adding 10-15 parts by weight of gallwood extract powder and mixing evenly, homogenizing under high pressure at 40-60 MPa for 2-4 times, concentrating under reduced pressure to 13-18% of the original weight, and then spray drying to obtain gallwood extract microcapsules;

[0013] Step III: Evenly mix 2-4 parts by weight of gallwood extract microcapsules, 3-6 parts by weight of corn starch and 1-2 parts by weight of microcrystalline cellulose, granulate, dry, and granulate, add 0.1-0.2 parts by weight of magnesium stearate and mix evenly, and then fill into hollow capsules to obtain the gallwood extract capsules.

[0014] Preferably, the weight ratio of the gallwood to the ethanol aqueous solution in step I is 1:10-15.

[0015] Preferably, the weight ratio of the extraction auxiliary material to the gallwood in step I is 1:8-10.

[0016] Preferably, the extraction auxiliary material in step I is glycerophosphorylcholine and / or 6-O-α-D-maltosyl-β-cyclodextrin.

[0017] Preferably, the extraction auxiliary material in step I is a mixture of glycerophosphorylcholine and 6-O-α-D-maltosyl-β-cyclodextrin in a weight ratio of 1-3:3.

[0018] The raw material used in the invention is the Chinese medicine gallwood, which is the branches and bark of the gallwood of the Rubiaceae family. The gallwood is washed, sliced, and dried for standby use, and the moisture content is within 8%. Gallwood is rich in various active ingredients, such as alkaloids, triterpenes, flavonoids, phenolic acid and saponin, etc., has the effects of clearing away heat and detoxifying, reducing swelling and relieving pain, and is suitable for treating colds and fever, acute tonsillitis, pharyngitis, bronchitis, pneumonia, urinary tract infection, enteritis, dysentery, cholecystitis and other diseases.

[0019] In the process of using ethanol and water as a mixed solvent to extract the gallwood extract, the invention significantly improves the extraction efficiency and biological activity of the gallwood extract by adding an extraction auxiliary material consisting of glycerophosphorylcholine and 6-O-α-D-maltosyl-β-cyclodextrin. Firstly, the functional groups such as phosphate groups and amino groups in the extraction auxiliary material glycerolphosphorylcholine can form hydrogen bonds with the hydroxyl groups on the surface of the gallwood cells, promote the dissolution of active ingredients such as phenols in the gallwood, and form hydrogen bonds with the hydroxyl groups on the gallwood cell wall to enhance the hydrophilicity of the cell wall, making its structure looser and increasing the permeability of the cell wall, which not only facilitates the penetration of the extraction solvent into the cell interior, but also promotes the release and diffusion of active ingredients in the cell, thereby improving the extraction efficiency; in addition, the amino group in glycerolphosphorylcholine carries a positive charge and can combine with the negatively charged gallwood cell cellulose and the like to change the electrical properties of the cell wall. This electrical change further enhances the permeability of the cell wall, allowing more active ingredients to be released from the cell; the positively charged amino group can also form electrostatic attraction with the negatively charged sites on the cell wall, further destroying the structure of the cell wall and promoting the release and diffusion of active ingredients. Secondly, the cyclodextrin structure in the extraction auxiliary material 6-O-α-D-maltosyl-β-cyclodextrin has an inclusion effect on the active ingredients such as triterpenes in the gallwood, which is helpful for the dissolution of the active ingredients. In addition, the active ingredients are wrapped and protected by the cavity structure of the cyclic oligosaccharide to prevent them from being damaged by high temperature and oxygen during the extraction process. As the heating proceeds, the solvent ethanol enters the gallwood cell tissue and boils violently from the inside, destroying the gallwood cell wall / membrane and causing the active ingredients to separate from the gallwood tissue. At this time, the cavity structure of 6-O-α-D-maltosyl-β-cyclodextrin can quickly wrap the released active ingredients, providing a protective barrier to prevent the active ingredients from decomposing or oxidizing at high temperatures, thereby effectively improving the extraction rate and stability of the active ingredients. It can be seen that the extraction excipients composed of glycerolphosphorylcholine and 6-O-α-D-maltosyl-β-cyclodextrin significantly improved the extraction efficiency and biological activity of the gallwood extract through the synergistic effect of the above-mentioned multiple mechanisms. Glycerolphosphorylcholine enhanced the permeability of the cell wall through hydrogen bonding and electrical changes, and promoted the release and diffusion of active ingredients; while 6-O-α-D-maltosyl-β-cyclodextrin, through the inclusion effect of its cavity structure, not only protected the active ingredients from high temperature and oxygen damage, but also ensured the efficient dissolution and stable preservation of the active ingredients during the extraction process, thereby maximally retaining the active ingredients in the gallwood and improving the quality and efficacy of the final gallwood extract capsules.

[0020] Preferably, the preparation method of the microcapsule wall material composite is:

[0021] Acetylated distarch phosphate is reacted with ozone to obtain oxidized starch phosphate; the oxidized starch phosphate is added into water for ultrasonic treatment, then L-theanine and 5-aminonicotinic acid are added, stirred for reaction, anhydrous ethanol is added to precipitate solid, filtered, washed, and freeze-dried to obtain modified grafted starch; the modified grafted starch, tamarind gum, and sodium caseinate are uniformly mixed to obtain a microcapsule wall material composite.

[0022] The microcapsule wall material composite used in the present invention is composed of homemade modified grafted starch, tamarind gum and sodium caseinate. The three components work synergistically to significantly improve the stability of the microcapsule structure and the coating and protection effect on the active ingredients of the gallwood extract. The carboxyl groups and antioxidant active structures in the modified grafted starch enhance the adsorption and protection of the active ingredients of the gallwood extract, while the addition of tamarind gum and sodium caseinate further strengthens the composite network structure of the wall material, improving the overall stability and mechanical strength of the microcapsule.

[0023] Furthermore, in the preparation process of the modified grafted starch, the present invention utilizes ozone to oxidize acetylated distarch phosphate to obtain a portion of converted carbonyl groups, and then adds L-theanine and 5-aminonicotinic acid, and utilizes the reaction between the amino group and the carbonyl group to graft the theanine / nicotinic acid active structure onto the starch molecular structure. This process not only gives the starch certain antioxidant properties, so that it can better protect the active ingredients of the gallwood extract coated therein as a wall material, but also introduces abundant carboxyl groups. These carboxyl groups have a stronger adsorption effect on the active ingredients in the gallwood extract, thereby more effectively realizing the coating protection of the active ingredients, extending the shelf life of the microcapsules, and improving the stability and bioavailability of the active ingredients in the gallwood extract.

[0024] It can be seen that the modified grafted starch and tamarind gum form a composite network structure through hydrogen bonding, and the electrostatic attraction between sodium caseinate and tamarind gum further strengthens the cross-linking degree of the network structure, making the network structure more compact. This ternary composite structure not only improves the overall stability of the microcapsule wall material, but also enhances the coating effect of the wall material on the active ingredients of the gallwood extract.

[0025] Preferably, the preparation method of the microcapsule wall material composite is:

[0026] Acetylated distarch phosphate is placed in an ozone generator, and a dry ozone reaction is performed for 0.3-1h under the condition of an ozone flow rate of 50-65L / h to obtain oxidized starch phosphate; 5-8 parts by weight of oxidized starch phosphate is added to 70-100 parts by weight of water, and ultrasonicated for 10-20min under the conditions of 20-30kHz and 100-200W, and then 0.2-0.4 parts by weight of L-theanine and 0.1-0.3 parts by weight of 5-aminonicotinic acid are added, and stirred for 4-6h under the conditions of 30-40°C and 200-500r / min, and then 150-180 parts by weight of anhydrous ethanol is added to precipitate solids, which are filtered, washed, and freeze-dried to obtain modified grafted starch; 2-3 parts by weight of modified grafted starch, 0.5-1-5 parts by weight of tamarind gum, and 1-2 parts by weight of sodium caseinate are evenly mixed to obtain a microcapsule wall material composite.

[0027] Preferably, the working parameters of the spray drying in step I are: the inlet air temperature is 160-180°C, and the outlet air temperature is 70-80°C.

[0028] Preferably, the average particle size D50 of the gallwood extract microcapsules in step II is 80-120 μm.

[0029] Preferably, the working parameters of the spray drying in step II are: the inlet air temperature is 175-185°C, and the outlet air temperature is 75-85°C.

[0030] Preferably, the granulation in step III uses 50-65wt% ethanol aqueous solution as a wetting agent, and the particle size of the granulated particles is 10-30 meshes.

[0031] Preferably, the capsules in step III have a filling weight of 0.3-0.5 g / capsule.

[0032] The present invention also provides a gallwood extract capsule, which is prepared by adopting the above production process.

[0033] Beneficial effects of the present invention:

[0034] The invention provides a production process of gallwood extract capsules, wherein the extraction step is optimized by adding specific extraction auxiliary materials glycerophosphorylcholine and / or 6-O-α-D-maltosyl-β-cyclodextrin, and the gallwood extract is microencapsulated by using a microcapsule wall material composite composed of modified grafted starch, tamarind gum and sodium caseinate, so that the biological activity of the gallwood extract is further improved, so that the gallwood extract has better heat-clearing and detoxifying and anti-inflammatory and analgesic effects, and the gallwood extract microcapsules have stable efficacy and high bioavailability. DETAILED DESCRIPTION

[0035] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0036] Example 1

[0037] A production process of gallwood extract capsules comprises the following steps:

[0038] Step I: grind the gallwood and pass it through a 100-mesh sieve, then add 76wt% ethanol aqueous solution and extraction auxiliary materials and mix them evenly, extract at 83°C for 90min, filter, repeat the extraction 3 times, combine the filtrates obtained 3 times, and decompress and concentrate the filtrates to 10% of the original weight to obtain gallwood extract; spray-dry the gallwood extract to obtain gallwood extract powder; the weight ratio of the gallwood to the ethanol aqueous solution is 1:12; the weight ratio of the extraction auxiliary materials to the gallwood is 1:9; the extraction auxiliary materials are a mixture of glycerophosphorylcholine (CAS: 28319-77-9) and 6-O-α-D-maltosyl-β-cyclodextrin (CAS: 104723-60-6) in a weight ratio of 2:3; wherein the working parameters of the spray drying are: the inlet air temperature is 170°C and the outlet air temperature is 75°C;

[0039] Step II: 3 parts by weight of the microcapsule wall material composite is added to 200 parts by weight of water, stirred at 300 r / min for 20 minutes, then 12 parts by weight of gallwood extract powder is added and mixed evenly, and high-pressure homogenization is performed at 50 MPa for 3 times. After the homogenization, the mixture is concentrated under reduced pressure to 15% of the original weight, and then spray-dried to obtain gallwood extract microcapsules with an average particle size D50 of 100 μm; wherein the working parameters of the spray drying are: the inlet air temperature is 180° C., and the outlet air temperature is 80° C.;

[0040] Step III: Mix 3 parts by weight of gallwood extract microcapsules, 4.5 parts by weight of corn starch and 1.5 parts by weight of microcrystalline cellulose, granulate with 60wt% ethanol aqueous solution as a wetting agent to a particle size of 20 mesh, dry, granulate, add 0.18 parts by weight of magnesium stearate and mix evenly, and then fill into hollow capsules with a filling amount of 0.4g / capsule to obtain the gallwood extract capsules.

[0041] The preparation method of the microcapsule wall material composite is as follows:

[0042] Acetylated distarch phosphate (CAS: 68130-14-3) is placed in an ozone generator, and a dry ozone reaction is carried out for 0.5 h at an ozone flow rate of 60 L / h to obtain oxidized starch phosphate; 6.5 parts by weight of oxidized starch phosphate is added to 80 parts by weight of water, and ultrasonicated at 20 kHz and 150 W for 15 min, and then 0.3 parts by weight of L-theanine and 0.2 parts by weight of 5-aminonicotinic acid are added, and stirred at 35° C. and 300 r / min for 5 h, and then 160 parts by weight of anhydrous ethanol is added to precipitate solids, which are filtered, washed, and freeze-dried to obtain modified grafted starch; 2.5 parts by weight of modified grafted starch, 1 part by weight of tamarind gum (CAS: 39386-78-2), and 1.5 parts by weight of sodium caseinate (CAS: 9005-46-3) are mixed uniformly to obtain a microcapsule wall material composite.

[0043] Example 2

[0044] A production process of gallwood extract capsules comprises the following steps:

[0045] Step I: grind the gallwood and pass it through a 100-mesh sieve, then add 76wt% ethanol aqueous solution and extraction auxiliary materials and mix them evenly, extract at 83°C for 90min, filter, repeat the extraction 3 times, combine the filtrates obtained 3 times, and decompress and concentrate the filtrates to 10% of the original weight to obtain gallwood extract; spray-dry the gallwood extract to obtain gallwood extract powder; the weight ratio of the gallwood to the ethanol aqueous solution is 1:12; the weight ratio of the extraction auxiliary materials to the gallwood is 1:9; the extraction auxiliary materials are glycerophosphorylcholine (CAS: 28319-77-9); wherein the working parameters of the spray drying are: the inlet air temperature is 170°C and the outlet air temperature is 75°C;

[0046] Step II: adding 3 parts by weight of the microcapsule wall material composite to 200 parts by weight of water, stirring at 300 r / min for 20 minutes, then adding 12 parts by weight of gallwood extract powder and mixing evenly, homogenizing under high pressure at 50 MPa for 3 times, concentrating under reduced pressure to 15% of the original weight after the end, and then spray drying to obtain gallwood extract microcapsules; wherein the working parameters of the spray drying are: the inlet air temperature is 180°C and the outlet air temperature is 80°C;

[0047] Step III: Mix 3 parts by weight of gallwood extract microcapsules, 4.5 parts by weight of corn starch and 1.5 parts by weight of microcrystalline cellulose, granulate with 60wt% ethanol aqueous solution as a wetting agent to a particle size of 20 mesh, dry, granulate, add 0.18 parts by weight of magnesium stearate and mix evenly, and then fill into hollow capsules with a filling amount of 0.4g / capsule to obtain the gallwood extract capsules.

[0048] The preparation method of the microcapsule wall material composite is as follows:

[0049] Acetylated distarch phosphate (CAS: 68130-14-3) is placed in an ozone generator, and a dry ozone reaction is carried out for 0.5 h at an ozone flow rate of 60 L / h to obtain oxidized starch phosphate; 6.5 parts by weight of oxidized starch phosphate is added to 80 parts by weight of water, and ultrasonicated at 20 kHz and 150 W for 15 min, and then 0.3 parts by weight of L-theanine and 0.2 parts by weight of 5-aminonicotinic acid are added, and stirred at 35° C. and 300 r / min for 5 h, and then 160 parts by weight of anhydrous ethanol is added to precipitate solids, which are filtered, washed, and freeze-dried to obtain modified grafted starch; 2.5 parts by weight of modified grafted starch, 1 part by weight of tamarind gum (CAS: 39386-78-2), and 1.5 parts by weight of sodium caseinate (CAS: 9005-46-3) are mixed uniformly to obtain a microcapsule wall material composite.

[0050] Example 3

[0051] A production process of gallwood extract capsules comprises the following steps:

[0052] Step I: grind the gallwood and pass it through a 100-mesh sieve, then add 76wt% ethanol aqueous solution and extraction auxiliary materials and mix them evenly, extract at 83°C for 90min, filter, repeat the extraction 3 times, combine the filtrates obtained 3 times, and decompress and concentrate the filtrates to 10% of the original weight to obtain gallwood extract; spray-dry the gallwood extract to obtain gallwood extract powder; the weight ratio of the gallwood to the ethanol aqueous solution is 1:12; the weight ratio of the extraction auxiliary materials to the gallwood is 1:9; the extraction auxiliary materials are 6-O-α-D-maltosyl-β-cyclodextrin (CAS: 104723-60-6); wherein the working parameters of the spray drying are: the inlet air temperature is 170°C and the outlet air temperature is 75°C;

[0053] Step II: adding 3 parts by weight of the microcapsule wall material composite to 200 parts by weight of water, stirring at 300 r / min for 20 minutes, then adding 12 parts by weight of gallwood extract powder and mixing evenly, homogenizing under high pressure at 50 MPa for 3 times, concentrating under reduced pressure to 15% of the original weight after the end, and then spray drying to obtain gallwood extract microcapsules; wherein the working parameters of the spray drying are: the inlet air temperature is 180°C and the outlet air temperature is 80°C;

[0054] Step III: Mix 3 parts by weight of gallwood extract microcapsules, 4.5 parts by weight of corn starch and 1.5 parts by weight of microcrystalline cellulose, granulate with 60wt% ethanol aqueous solution as a wetting agent to a particle size of 20 mesh, dry, granulate, add 0.18 parts by weight of magnesium stearate and mix evenly, and then fill into hollow capsules with a filling amount of 0.4g / capsule to obtain the gallwood extract capsules.

[0055] The preparation method of the microcapsule wall material composite is as follows:

[0056] Acetylated distarch phosphate (CAS: 68130-14-3) is placed in an ozone generator, and a dry ozone reaction is carried out for 0.5 h at an ozone flow rate of 60 L / h to obtain oxidized starch phosphate; 6.5 parts by weight of oxidized starch phosphate is added to 80 parts by weight of water, and ultrasonicated at 20 kHz and 150 W for 15 min, and then 0.3 parts by weight of L-theanine and 0.2 parts by weight of 5-aminonicotinic acid are added, and stirred at 35° C. and 300 r / min for 5 h, and then 160 parts by weight of anhydrous ethanol is added to precipitate solids, which are filtered, washed, and freeze-dried to obtain modified grafted starch; 2.5 parts by weight of modified grafted starch, 1 part by weight of tamarind gum (CAS: 39386-78-2), and 1.5 parts by weight of sodium caseinate (CAS: 9005-46-3) are mixed uniformly to obtain a microcapsule wall material composite.

[0057] Example 4

[0058] A production process of gallwood extract capsules comprises the following steps:

[0059] Step I: grind the gallwood and pass it through a 100-mesh sieve, then add 76wt% ethanol aqueous solution and extraction auxiliary materials and mix them evenly, extract at 83°C for 90min, filter, repeat the extraction 3 times, combine the filtrates obtained 3 times, and decompress and concentrate the filtrates to 10% of the original weight to obtain gallwood extract; spray-dry the gallwood extract to obtain gallwood extract powder; the weight ratio of the gallwood to the ethanol aqueous solution is 1:12; the weight ratio of the extraction auxiliary materials to the gallwood is 1:9; the extraction auxiliary materials are a mixture of glycerophosphorylcholine (CAS: 28319-77-9) and 6-O-α-D-maltosyl-β-cyclodextrin (CAS: 104723-60-6) in a weight ratio of 2:3; wherein the working parameters of the spray drying are: the inlet air temperature is 170°C and the outlet air temperature is 75°C;

[0060] Step II: adding 3 parts by weight of the microcapsule wall material composite to 200 parts by weight of water, stirring at 300 r / min for 20 minutes, then adding 12 parts by weight of gallwood extract powder and mixing evenly, homogenizing under high pressure at 50 MPa for 3 times, concentrating under reduced pressure to 15% of the original weight after the end, and then spray drying to obtain gallwood extract microcapsules; wherein the working parameters of the spray drying are: the inlet air temperature is 180°C and the outlet air temperature is 80°C;

[0061] Step III: Mix 3 parts by weight of gallwood extract microcapsules, 4.5 parts by weight of corn starch and 1.5 parts by weight of microcrystalline cellulose, granulate with 60wt% ethanol aqueous solution as a wetting agent to a particle size of 20 mesh, dry, granulate, add 0.18 parts by weight of magnesium stearate and mix evenly, and then fill into hollow capsules with a filling amount of 0.4g / capsule to obtain the gallwood extract capsules.

[0062] The preparation method of the microcapsule wall material composite is as follows:

[0063] 2.5 parts by weight of sodium starch octenylsuccinate (CAS: 66829-29-6), 1 part by weight of tamarind gum (CAS: 39386-78-2), and 1.5 parts by weight of sodium caseinate (CAS: 9005-46-3) were mixed evenly to obtain a microcapsule wall material composite.

[0064] Example 5

[0065] A production process of gallwood extract capsules comprises the following steps:

[0066] Step I: grind the gallwood and pass it through a 100-mesh sieve, then add 76wt% ethanol aqueous solution and extraction auxiliary materials and mix them evenly, extract at 83°C for 90min, filter, repeat the extraction 3 times, combine the filtrates obtained 3 times, and decompress and concentrate the filtrates to 10% of the original weight to obtain gallwood extract; spray-dry the gallwood extract to obtain gallwood extract powder; the weight ratio of the gallwood to the ethanol aqueous solution is 1:12; the weight ratio of the extraction auxiliary materials to the gallwood is 1:9; the extraction auxiliary materials are a mixture of glycerophosphorylcholine (CAS: 28319-77-9) and 6-O-α-D-maltosyl-β-cyclodextrin (CAS: 104723-60-6) in a weight ratio of 2:3; wherein the working parameters of the spray drying are: the inlet air temperature is 170°C and the outlet air temperature is 75°C;

[0067] Step II: adding 3 parts by weight of the microcapsule wall material composite to 200 parts by weight of water, stirring at 300 r / min for 20 minutes, then adding 12 parts by weight of gallwood extract powder and mixing evenly, homogenizing under high pressure at 50 MPa for 3 times, concentrating under reduced pressure to 15% of the original weight after the end, and then spray drying to obtain gallwood extract microcapsules; wherein the working parameters of the spray drying are: the inlet air temperature is 180°C and the outlet air temperature is 80°C;

[0068] Step III: Mix 3 parts by weight of gallwood extract microcapsules, 4.5 parts by weight of corn starch and 1.5 parts by weight of microcrystalline cellulose, granulate with 60wt% ethanol aqueous solution as a wetting agent to a particle size of 20 mesh, dry, granulate, add 0.18 parts by weight of magnesium stearate and mix evenly, and then fill into hollow capsules with a filling amount of 0.4g / capsule to obtain the gallwood extract capsules.

[0069] The preparation method of the microcapsule wall material composite is as follows:

[0070] Acetylated distarch phosphate (CAS: 68130-14-3) was placed in an ozone generator, and a dry ozone reaction was carried out for 0.5 h under the condition of an ozone flow rate of 60 L / h to obtain oxidized starch phosphate; 2.5 parts by weight of oxidized starch phosphate, 1 part by weight of tamarind gum (CAS: 39386-78-2), and 1.5 parts by weight of sodium caseinate (CAS: 9005-46-3) were mixed uniformly to obtain a microcapsule wall material composite.

[0071] Example 6

[0072] A production process of gallwood extract capsules comprises the following steps:

[0073] Step I: grind the gallwood and pass it through a 100-mesh sieve, then add 76wt% ethanol aqueous solution and extraction auxiliary materials and mix them evenly, extract at 83°C for 90min, filter, repeat the extraction 3 times, combine the filtrates obtained 3 times, and decompress and concentrate the filtrates to 10% of the original weight to obtain gallwood extract; spray-dry the gallwood extract to obtain gallwood extract powder; the weight ratio of the gallwood to the ethanol aqueous solution is 1:12; the weight ratio of the extraction auxiliary materials to the gallwood is 1:9; the extraction auxiliary materials are a mixture of glycerophosphorylcholine (CAS: 28319-77-9) and 6-O-α-D-maltosyl-β-cyclodextrin (CAS: 104723-60-6) in a weight ratio of 2:3; wherein the working parameters of the spray drying are: the inlet air temperature is 170°C and the outlet air temperature is 75°C;

[0074] Step II: adding 3 parts by weight of the microcapsule wall material composite to 200 parts by weight of water, stirring at 300 r / min for 20 minutes, then adding 12 parts by weight of gallwood extract powder and mixing evenly, homogenizing under high pressure at 50 MPa for 3 times, concentrating under reduced pressure to 15% of the original weight after the end, and then spray drying to obtain gallwood extract microcapsules; wherein the working parameters of the spray drying are: the inlet air temperature is 180°C and the outlet air temperature is 80°C;

[0075] Step III: Mix 3 parts by weight of gallwood extract microcapsules, 4.5 parts by weight of corn starch and 1.5 parts by weight of microcrystalline cellulose, granulate with 60wt% ethanol aqueous solution as a wetting agent to a particle size of 20 mesh, dry, granulate, add 0.18 parts by weight of magnesium stearate and mix evenly, and then fill into hollow capsules with a filling amount of 0.4g / capsule to obtain the gallwood extract capsules.

[0076] The preparation method of the microcapsule wall material composite is as follows:

[0077] Acetylated distarch phosphate (CAS: 68130-14-3) is placed in an ozone generator, and a dry ozone reaction is carried out for 0.5 h at an ozone flow rate of 60 L / h to obtain oxidized starch phosphate; 6.5 parts by weight of oxidized starch phosphate are added to 80 parts by weight of water, and ultrasonicated at 20 kHz and 150 W for 15 min, and then 0.3 parts by weight of L-theanine and 0.2 parts by weight of 5-aminonicotinic acid are added, and stirred at 35° C. and 300 r / min for 5 h, and then 160 parts by weight of anhydrous ethanol is added to precipitate solids, which are filtered, washed, and freeze-dried to obtain modified grafted starch; 2.5 parts by weight of modified grafted starch and 2.5 parts by weight of sodium caseinate (CAS: 9005-46-3) are mixed evenly to obtain a microcapsule wall material composite.

[0078] Test Example 1

[0079] The coverage rate of the gallwood extract microcapsules obtained in the above example was determined by solvent extraction method. Wherein, coverage rate = weight of coated core material / total weight of microcapsules × 100%. The test results are shown in Table 1.

[0080] Table 1: Coverage test results

[0081]

[0082] Test Example 2

[0083] Kunming mice weighing 20-30g were used as test subjects and randomly divided into 9 groups, each group had 10 mice, half of which were male and half were female. Kunming mice were gavaged with the gallwood extract microcapsules obtained in the above embodiment (three doses of 0.1g / kg, 0.2g / kg, and 0.4g / kg) once a day for 1 week; the blank control group was gavaged with normal saline (0.2g / kg) once a day; the aspirin group was gavaged with aspirin (0.2g / kg) once a day. 1h after administration on the 7th day, 40μL of xylene was applied to the left auricle of each mouse to cause mouse ear swelling, and the middle part of the right ear of the mouse was marked. After 40min, the mouse was killed by dislocating the neck, weighed, and the ears were quickly cut off. After aligning the ear edges, holes were punched with a puncher, and the mass of the left and right ear pieces was quickly weighed and the ear swelling degree (mg) was calculated, thereby obtaining the swelling inhibition percentage. The gallwood extract capsules obtained in the above example were stored at room temperature and protected from light for 6 months, and then tested again according to the above test method. Wherein, the swelling inhibition percentage = (ear swelling degree of the blank control group - ear swelling degree of the experimental group) / ear swelling degree of the blank control group × 100%. The test results are shown in Tables 2 and 3.

[0084] Table 2: Initial anti-inflammatory efficacy test results

[0085]

[0086] Table 3: Anti-inflammatory efficacy test results after 6 months

[0087]

[0088] As can be seen from Tables 1-3, the gallwood extract capsule obtained in Example 1 of the present invention has the best active efficacy and stability. Compared with Examples 2-3, Example 1 uses glycerylphosphorylcholine and 6-O-α-D-maltosyl-β-cyclodextrin as the extraction auxiliary materials, and the two cooperate with each other to significantly improve the biological activity of the gallwood extract. Glycerylphosphorylcholine enhances the permeability of the cell wall through hydrogen bonding and electrical changes, and promotes the release and diffusion of active ingredients, while 6-O-α-D-maltosyl-β-cyclodextrin, through the inclusion effect of its cavity structure, not only protects the active ingredients from high temperature and oxygen damage, but also ensures the efficient dissolution and stable preservation of the active ingredients during the extraction process, and retains the active ingredients in the gallwood to the maximum extent, and improves the quality and efficacy of the final gallwood extract capsule. Compared with Examples 4-6, Example 1 uses specific modified grafted starch, tamarind gum and sodium caseinate to form a microcapsule wall material. The modified grafted starch and tamarind gum form a composite network structure through hydrogen bonding. The electrostatic attraction between sodium caseinate and tamarind gum further strengthens the cross-linking degree of the network structure, making the network structure more compact. At the same time, the carboxyl groups and antioxidant active structures in the modified grafted starch enhance the adsorption and protection of the active ingredients of the gallwood extract. This ternary composite structure not only improves the overall stability of the microcapsule wall material, but also enhances the coating effect of the wall material on the active ingredients of the gallwood extract.

[0089] The preferred specific embodiments of the present invention are described in detail above. It should be understood that a person skilled in the art can make many modifications and changes based on the concept of the present invention without creative work. Therefore, any technical solution that can be obtained by a person skilled in the art through logical analysis, reasoning or limited experiments based on the concept of the present invention on the basis of the prior art should be within the scope of protection determined by the claims.

Claims

1. A production process for Gallwood Extract Capsules, characterized in that: The following steps are involved: Step I: crush the gallwood and sieve it, then add ethanol water solution and extraction auxiliary materials to mix evenly, heat extraction, filter, repeat extraction 2-4 times, combine the filtrate, and concentrate under reduced pressure to obtain gallwood extract; spray dry the gallwood extract to obtain gallwood extract powder; the extraction auxiliary materials are glycerylphosphorylcholine and / or 6-O-α-D-maltosyl-β-cyclodextrin; Step II: adding the microcapsule wall material composite into water and stirring, then adding the gallwood extract powder and mixing evenly, high pressure homogenization, and then concentrating under reduced pressure, and then spray drying to obtain gallwood extract microcapsules; Step III: uniformly mix the gallwood extract microcapsules, corn starch and microcrystalline cellulose, granulate, dry, and granulate, add magnesium stearate and mix evenly, and then fill into hollow capsules to obtain the gallwood extract capsules.

2. The production process of the Gallwood Extract Capsules according to claim 1, characterized in that: The microcapsule wall material composite in step II is prepared from modified grafted starch, tamarind gum and sodium caseinate.

3. The production process of the Gallwood Extract Capsule according to claim 1, characterized in that: The preparation method of the microcapsule wall material composite in step II is: Acetylated distarch phosphate is reacted with ozone to obtain oxidized starch phosphate; the oxidized starch phosphate is added into water for ultrasonic treatment, then L-theanine and 5-aminonicotinic acid are added, stirred for reaction, anhydrous ethanol is added to precipitate solid, filtered, washed, and freeze-dried to obtain modified grafted starch; the modified grafted starch, tamarind gum, and sodium caseinate are uniformly mixed to obtain a microcapsule wall material composite.

4. The production process of the Gallwood Extract Capsule according to claim 1, characterized in that: The extraction auxiliary material in step I is a mixture of glycerolphosphorylcholine and 6-O-α-D-maltosyl-β-cyclodextrin.

5. The production process of the Gallwood Extract Capsule according to claim 1, characterized in that: The following steps are involved: Step I: crush the gallwood and pass it through an 80-150 mesh sieve, then add 75-78wt% ethanol aqueous solution and extraction auxiliary materials and mix them evenly, extract at 80-85°C for 80-100 minutes, filter, repeat the extraction 2-4 times, combine the obtained filtrate, and reduce the pressure to concentrate the filtrate to 8-12% of the original weight to obtain gallwood extract; spray dry the gallwood extract to obtain gallwood extract powder; Step II: adding 2-4 parts by weight of the microcapsule wall material composite to 180-220 parts by weight of water, stirring at 200-500 r / min for 10-30 min, then adding 10-15 parts by weight of gallwood extract powder and mixing evenly, homogenizing under high pressure at 40-60 MPa for 2-4 times, concentrating under reduced pressure to 13-18% of the original weight, and then spray drying to obtain gallwood extract microcapsules; Step III: Evenly mix 2-4 parts by weight of gallwood extract microcapsules, 3-6 parts by weight of corn starch and 1-2 parts by weight of microcrystalline cellulose, granulate, dry, and granulate, add 0.1-0.2 parts by weight of magnesium stearate and mix evenly, and then fill into hollow capsules to obtain the gallwood extract capsules.

6. The production process of the Gallwood Extract Capsules according to claim 1, characterized in that: The weight ratio of the gallwood to the ethanol aqueous solution in step I is 1:10-15.

7. The production process of the Gallwood Extract Capsules according to claim 1, characterized in that: The weight ratio of the extraction auxiliary material to the gallwood in step I is 1:8-10.

8. The production process of the Gallwood Extract Capsule according to claim 1, characterized in that: The average particle size D50 of the gallwood extract microcapsules in step II is 80-120 μm.

9. The production process of Gallwood Extract Capsules according to claim 1, characterized in that: The filling amount of each capsule in step III is 0.3-0.5 g / capsule.

10. A gallwood extract capsule, characterized in that: The method is obtained by adopting the production process described in any one of claims 1 to 9.

Images