CN113908227A - Oral liquid and preparation method thereof - Google Patents

Oral liquid and preparation method thereof Download PDF

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Publication number
CN113908227A
CN113908227A CN202111149361.9A CN202111149361A CN113908227A CN 113908227 A CN113908227 A CN 113908227A CN 202111149361 A CN202111149361 A CN 202111149361A CN 113908227 A CN113908227 A CN 113908227A
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CN
China
Prior art keywords
parts
prepared
oral liquid
biochar
water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202111149361.9A
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Chinese (zh)
Inventor
蒋建龙
蒋庞彪
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Suzhou Huabao Pharmaceutical Co ltd
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Suzhou Huabao Pharmaceutical Co ltd
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Filing date
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Application filed by Suzhou Huabao Pharmaceutical Co ltd filed Critical Suzhou Huabao Pharmaceutical Co ltd
Priority to CN202111149361.9A priority Critical patent/CN113908227A/en
Publication of CN113908227A publication Critical patent/CN113908227A/en
Pending legal-status Critical Current

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Abstract

The invention discloses an oral liquid and a preparation method thereof. The preparation method of the oral liquid comprises the following steps: the oral liquid for the growth of the spring treasure is prepared by processing ginseng, alisma orientale, prepared fleece-flower root, angelica, schisandra chinensis, eucommia ulmoides, rhizoma anemarrhenae, phellodendron, medlar, Chinese yam, asparagus cochinchinensis, fructus psoraleae, rhizoma curculiginis, parasitic loranthus, radix ophiopogonis, glossy privet fruit, rehmannia glutinosa, eclipta, prepared rehmannia root, achyranthes bidentata, salvia miltiorrhiza, poria cocos, morinda officinalis, epimedium herb and astragalus mongholicus by percolation, decoction and modified charcoal adsorption technology, wherein the modified charcoal is prepared by carbonizing traditional Chinese medicine residues and adding calcium chloride, ferric chloride and silicon dioxide for modification. Compared with the prior art, the oral liquid prepared by the invention has the advantages of antianaphylaxis, low toxicity and easy storage.

Description

Oral liquid and preparation method thereof
Technical Field
The invention relates to the field of oral liquid, in particular to oral liquid and a preparation method thereof.
Background
Changchunbao oral liquid is prepared with 25 kinds of Chinese medicinal materials, including ginseng, wolfberry fruit, schisandra, angelica, tuckahoe, privet fruit, etc. and has the functions of strengthening immunity, nourishing liver, protecting stomach, invigorating Qi and blood, regulating Yin and Yang and strengthening physique. Is used for treating asthenia of middle aged and elderly people, and symptoms caused by liver and kidney deficiency, such as listlessness, dizziness, soreness of waist and legs, dim eyesight, tinnitus, amnesia, insomnia, palpitation, short breath, edema, and nocturia; can also be used for adjuvant treatment of hypertension patients with hyperlipidemia. Collected in the eleventh volume of the Chinese patent medicine prescription preparation recorded in the ministry of health drug Standard.
Chinese patent CN1368251A discloses a nano Changchunbao preparation, which is prepared from nano ginseng, nano wolfberry fruit, nano yam, nano schisandra fruit, nano asparagus root, nano ophiopogon root, nano rehmannia root, nano prepared fleece flower root, nano poria, nano achyranthes root, nano angelica, nano psoralea fruit, nano eucommia bark, nano morinda root, nano anemarrhena rhizome, nano phellodendron, nano curculigo rhizome, nano epimedium, nano alisma rhizome, nano red sage root, nano astragalus root, nano mistletoe, nano ligustrum japonicum and nano eclipta by proportioning to prepare a new medicinal preparation, wherein the particle fineness of the medicinal preparation reaches 1200 meshes and 1500 meshes, the particle size is 0.1-200nm, the majority of the particle size is less than 100nm, and the medicinal preparation has new physical properties. It is prepared through microwave extraction, decompression concentration, spray drying in supersonic jet and other steps. The medicine has high bioavailability and remarkable therapeutic effect. However, the nanometer Chinese herbal medicine adopted by the invention is finally purified to obtain the extract, so that the waste of the working procedure exists, and the practicability is not realized.
The invention patent with publication number CN107998276A discloses a Changchun bao oral liquid, which is composed of the following raw materials in parts by weight: 15 parts of ginseng, 10 parts of medlar, 8 parts of Chinese yam, 5 parts of five gourmet seeds, 4 parts of asparagus, 2 parts of dwarf lilyturf tuber, 6 parts of rehmannia root, 10 parts of tuber fleeceflower root, 5 parts of tuckahoe, 3 parts of achyranthes root, 5 parts of angelica, 4 parts of malaytea scurfpea fruit, 3 parts of eucommia bark, 6 parts of morinda officinalis, 5 parts of rhizoma anemarrhenae, 7 parts of phellodendron, 5 parts of curculigo orchioides, 10 parts of epimedium, 3 parts of oriental waterplantain rhizome, 7 parts of salvia miltiorrhiza, 12 parts of astragalus root, 4 parts of parasitic loranthus, 3 parts of glossy privet fruit and 8 parts of yerbadetajo herb. The method is a simple improvement of extraction process, has complicated process, has no obvious improvement on the curative effect and function of Changchunbao oral liquid, and has more toxic components.
Disclosure of Invention
In view of the defects of complicated preparation procedures, loss of toxic components and effective components, storage and deterioration in the prior art, the technical problem to be solved by the invention is to construct an anti-allergic, low-toxicity and easy-to-store Changchunbao oral liquid by adopting a modified charcoal filtering mode.
In order to realize the purpose, the invention provides a preparation method of Changchunbao oral liquid, which comprises the following steps:
step 1, grinding ginseng, rhizoma alismatis, prepared polygonum multiflorum, angelica, schisandra chinensis and eucommia ulmoides respectively, and sieving by adopting a 50-200-mesh sieve; then, soaking the ginseng powder in 20-40 wt% ethanol water solution serving as a solvent, mixing the alisma orientale powder, the prepared polygonum multiflorum powder, the angelica powder, the schisandra chinensis powder and the eucommia ulmoides powder in 60-80 wt% ethanol water solution serving as a solvent for 5-20 hours, percolating, collecting percolate, and preparing adult ginseng percolate and mixed percolate;
step 2, adding water into rhizoma anemarrhenae, cortex phellodendri, fructus lycii, Chinese yam, radix asparagi, fructus psoraleae, rhizoma curculiginis, parasitic loranthus, radix ophiopogonis, glossy privet fruit, rehmannia glutinosa, herba ecliptae, prepared rehmannia root, radix achyranthis bidentatae, radix salviae miltiorrhizae, poria cocos, morinda officinalis, herba epimedii and radix astragali, decocting for two times, adding water for the first time, decocting for 1-3 hours, collecting decoction, adding water for the second time, decocting for 1-3 hours, and collecting decoction; mixing the two decoctions, filtering by adopting a filter screen of 50-200 meshes, then evaporating and concentrating until the relative density is 1.06-1.09 at 65 ℃, the evaporation temperature is 60-70 ℃, adding 1-3 times of anhydrous ethanol by mass, stirring uniformly, standing for 5-15 h, and taking supernatant;
step 3, adding the mixed percolate prepared in the step 1 into the supernatant in the step 2, stirring uniformly, standing for 10-30 h, and taking the mixed supernatant for later use; and adding stevioside into the ginseng percolate prepared in the step 1, uniformly mixing, adding sodium benzoate, ethylparaben and mixed supernatant, uniformly stirring, boiling, adding modified biochar under the boiling condition, performing centrifugal filtration at the centrifugal speed of 12000-15000 r/min for 5-20 min, collecting the centrifugal liquid, filtering the centrifugal liquid by using a 0.1-1 mu m nylon membrane, collecting filtrate, adding water to prepare 500-1500 mL of solution, and uniformly stirring to obtain the periwinkle oral liquid.
Preferably, the components in the step 1 are calculated by weight parts: 10-20 parts of ginseng, 20-30 parts of rhizoma alismatis, 20-30 parts of prepared polygonum multiflorum, 12-20 parts of angelica sinensis, 5-12 parts of schisandra chinensis, 8-15 parts of eucommia ulmoides, 50-150 parts of 20-40 wt% ethanol water solution and 300-500 parts of 60-80 wt% ethanol water solution.
Preferably, the percolation method adopted in the step 1 is one of a single percolation method, a double percolation method, a pressure percolation method and a counter-current percolation method.
Preferably, the components in the step 2 are calculated by weight parts: 8-15 parts of rhizoma anemarrhenae, 8-15 parts of cortex phellodendri, 10-20 parts of fructus lycii, 5-15 parts of Chinese yam, 10-20 parts of radix asparagi, 10-20 parts of bone fat supplementing, 5-12 parts of rhizoma curculiginis, 10-20 parts of parasitic loranthus, 10-20 parts of radix ophiopogonis, 15-25 parts of glossy privet fruit, 10-20 parts of rehmannia, 15-25 parts of herba ecliptae, 10-20 parts of prepared rehmannia root, 10-20 parts of radix achyranthis bidentatae, 10-20 parts of radix salviae miltiorrhizae, 10-20 parts of poria cocos, 10-20 parts of morinda officinalis, 5-12 parts of herba epimedii, 10-20 parts of radix astragali, 1400-2000 parts of water for the first time and 1000-1500 parts of water for the second time.
Preferably, the components in the step 3 are calculated by weight parts: 30-50 parts of the supernatant in the step 2, 20-30 parts of the mixed percolate prepared in the step 1, 0.5-2 parts of steviosin, 10-20 parts of the ginseng percolate prepared in the step 1, 1-5 parts of sodium benzoate, 0.1-0.5 part of ethylparaben, 40-60 parts of the mixed supernatant and 10-30 parts of modified biochar.
Preferably, the modified biochar in the step 3 is prepared by the following steps:
s1, rinsing the fructus forsythiae residues, the corn straw residues and the honeysuckle residues with water, and drying at 70-90 ℃ for 10-30 hours; then crushing, sieving by using a 50-200 mesh sieve, and collecting residue powder; carbonizing the residue powder at a high temperature of 400-600 ℃ for 0.5-2 h to obtain biochar;
s2, repeatedly washing the biochar prepared in the step S1 with water until the pH value of the washing water is neutral, and drying the biochar in an oven at 70-90 ℃ for 20-30 hours to obtain dried biochar; adding calcium chloride, ferric chloride, silicon dioxide and water into the dried biochar, mixing, and stirring for 0.5-2 h; and then putting the mixture into a high-temperature environment, heating the mixture to 400-600 ℃ at a speed of 5-15 ℃/min, preserving the heat at 400-600 ℃ for 50-150 min, rinsing the mixture by using 0.01-0.5 mol/L hydrochloric acid, washing the rinsed mixture by using water until the pH value of a washing solution is neutral, drying the rinsed mixture for 10-30 h at 70-90 ℃, grinding the rinsed mixture, and sieving the ground mixture by using a 50-200-mesh sieve to prepare the modified biochar.
Preferably, in the step S1, the components are calculated by weight: 10-30 parts of fructus forsythiae residues, 5-15 parts of corn straw residues and 10-20 parts of honeysuckle flower residues.
Preferably, in the step S2, the components are calculated by weight: 10-20 parts of the biochar prepared in the step S1, 5-15 parts of dried biochar, 10-20 parts of calcium chloride, 5-15 parts of ferric chloride, 1-6 parts of silicon dioxide, 70-100 parts of water and 100-300 parts of 0.01-0.5 mol/L hydrochloric acid.
Biochar is a product of pyrolysis of biomass under high temperature, high pressure and anaerobic conditions, the biomass type and pyrolysis conditions have an effect on the specific surface area and pore structure of the biochar, and biochar extracted from different raw materials can be successfully used for the removal of antibiotics and allergens. The biochar has a good pore structure and strong adsorption capacity, and is beneficial to improving the cell density and the microbial permeability. Meanwhile, the biochar is recommended as a carrier material, and has the advantages of good mass transfer, no toxicity to cells, high chemical stability, low cost, simplicity in preparation and the like. Taking cotton hull biochar as an example, the cotton hull biochar modified by phosphoric acid has good adsorption performance on sulfadiazine and can be recycled for multiple times. After the silicon dioxide particles are added into the biomass bamboo, the total pore volume and the pore diameter of the silicon dioxide composite biochar are both obviously improved, and the adsorption capacity of the biochar on allergens and toxic components is greatly improved. In addition, the biochar prepared from rice straws, camphor leaves and pine wood is also applied to removal of harmful substances in water. In the existing research, there are few reports of extracting biochar from Chinese herbal medicine residues.
The traditional Chinese medicine is a treasure in China and has obvious curative effect on treating global diseases. From the perspective of low carbon economy, the utilization of Chinese herbal medicine residues to prepare biochar can improve the availability of materials and reduce the influence on the environment. Because the Chinese herbal medicines are various in variety, the biochar prepared from different materials has different adsorption characteristics and different preparation processes.
After long-term administration of the traditional Chinese medicine containing the polygonum multiflorum or the prepared polygonum multiflorum, liver cells can have edema, steatosis, partial punctate necrosis, balloon-like degeneration and vacuole-like degeneration with different degrees, and some animals have the phenomena of central vein inflammatory cell focal infiltration, liver tissue focal necrosis and the like, so that liver injury is mainly related to oxidative phosphorylation of mitochondrial functions and abnormal conduction of TCA circulation signal pathways. When the NADH deaminase family is abnormally expressed and the phenylalanine metabolism is abnormally, the function of oxidative phosphorylation is disordered, the function of mitochondria is damaged, and the apoptosis is caused, and the components causing the function can be related to anthraquinone compounds (especially emodin and derivatives thereof).
The residues of fructus forsythiae, corn stalks and honeysuckle are selected as the source of the biochar, the biochar prepared from the residues has a developed pore structure, and the biochar has stronger adsorption capacity due to rich open pores and functional groups on the surface, so that the content of allergens and anthraquinone toxic components in Chinese herbal medicines can be reduced, and the adsorption capacity of the biochar is improved by modifying the biochar by adopting calcium chloride, ferric chloride and silicon dioxide. The specific surface area of the modified biochar is greatly increased, and calcium, iron and chloride ions are attached to the biochar. Ca2+The presence of (A) neutralizes anions on the surface of the biochar, reducing electrostatic repulsion. A microporous adsorbent is constructed. Because more allergens and toxic components are generated in the processing and storage processes of the Chinese herbal medicines, the allergens, the toxic components and the unstable components influence the efficacy and the storage time of the Changchunbao oral liquid, compared with other biochar, the modified biochar has obvious advantages of adsorbing the allergens and the toxic components of the Chinese herbal medicines, reducing anaphylactic reaction, reducing toxic substances and prolonging the quality guarantee period of the oral liquid. During the adsorption process at high temperature, high temperature can provide a large amount of energy, the traditional Chinese medicine extract is easy to diffuse at higher temperature, the adsorption amount of the modified biochar is greatly increased at high temperature, and metal salt ions Ca on the biochar2+Electrostatic repulsion can be attenuated. The oxygen-containing functional groups on the molecule can be bound to the biochar surface through hydrogen bonds. The functional groups such as hydroxyl and amine in toxic and unstable components can be combined with hydroxyl and carboxyl on biocharThe radicals form hydrogen bonds, enhancing the adsorption of toxic and unstable components.
Due to the adoption of the technical scheme, compared with the prior art, the Changchunbao oral liquid and the preparation method thereof have the advantages that: 1) the adsorption effect of the modified charcoal can reduce the content of allergen and reduce anaphylactic reaction. 2) The unstable components and toxic components in the Changchunbao oral liquid are removed through adsorption, the efficacy of the effective components is maintained, and the shelf life is prolonged. 3) The preparation process is safe and environment-friendly, and the product quality is stable.
Detailed Description
Sources of the main raw materials in the examples:
the residues of fructus forsythiae, corn stalk and honeysuckle are all from Shandong Baihe limited biotechnology company.
Ginseng: county, Liaoning province.
Schisandra chinensis and rhizoma anemarrhenae: the producing area is Hebei Tangshan.
Phellodendron bark: the four rivers of the production area are both rivers.
Wolfberry fruit: produced in Ningxia Hui nationality Zhongning county.
Prepared fleece-flower root, Chinese angelica, yam, asparagus, psoralea fruit, curculigo orchioides, alisma orientale and Chinese taxillus twig: the origin is Sichuan Tongjiang county.
Alisma orientale, Fangji province, Jianou City. The rhizoma alismatis adopted in the embodiment of the invention is processed rhizoma alismatis, and the specific processing method comprises the following steps: removing impurities, slicing, drying, placing in a parching container, heating with slow fire, parching to slight yellow, taking out, and cooling.
Eucommia ulmoides: the province of Hunan province. The eucommia ulmoides adopted in the embodiment of the invention is the eucommia ulmoides after being processed, and the specific processing method comprises the following steps: removing impurities, scraping residual coarse skin, cleaning, shredding, drying, parching with middle fire until the shred is broken and the surface is brown, taking out, spreading and drying in the air, and cooling thoroughly.
Radix ophiopogonis and glossy privet fruit: the origin is Zhejiang Dongyang city.
Rehmannia root, eclipta: liaoning Dandong in the area of birth.
Prepared rehmannia root, achyranthes and red sage root: the Henan Lin city of origin.
Tuckahoe, poria cocos: the Yunan Wenshan Zhuang seedling family in the producing area is autonomous.
Morinda officinalis: ou City of Ou province, Fujian province.
Herba epimedii and radix astragali: gansu Min county of origin.
Example 1
The preparation method of the Changchunbao oral liquid comprises the following steps of:
step 1, respectively crushing 16 parts of ginseng, 24 parts of rhizoma alismatis, 24 parts of prepared polygonum multiflorum, 16 parts of angelica, 8 parts of schisandra chinensis and 11 parts of eucommia ulmoides by using a grinder, and sieving by using a 100-mesh sieve; then, 100 parts of 30 wt% ethanol water solution of ginseng is used as a solvent, and 400 parts of 70 wt% ethanol water solution of rhizoma alismatis powder, prepared polygonum multiflorum powder, angelica powder, schisandra chinensis powder and eucommia ulmoides powder are mixed and then used as a solvent, after the mixture is soaked for 12 hours, single percolation is carried out, the outflow rate of percolate is 2mL/min, and the percolate is collected to prepare the ginseng percolate for adults and mixed percolate;
step 2, adding water into 12 parts of rhizoma anemarrhenae, 12 parts of cortex phellodendri, 16 parts of fructus lycii, 11 parts of Chinese yam, 16 parts of radix asparagi, 16 parts of fructus psoraleae, 8 parts of rhizoma curculiginis, 16 parts of parasitic loranthus, 16 parts of radix ophiopogonis, 19 parts of glossy privet fruit, 16 parts of rehmannia, 19 parts of herba ecliptae, 16 parts of prepared rehmannia root, 16 parts of radix achyranthis bidentatae, 16 parts of salvia miltiorrhiza, 16 parts of poria cocos, 16 parts of radix morindae officinalis, 8 parts of herba epimedii and 16 parts of radix astragali for decoction twice, adding 1600 parts of water for the first time, decocting for 2 hours, and collecting decoction; adding 1200 parts of water for the second time, decocting for 2 hours, collecting decoction, mixing the decoction obtained in the two times, filtering by adopting a 100-mesh filter screen, then carrying out evaporation concentration until the relative density is 1.06-1.09 at 65 ℃, the evaporation temperature is 65 ℃, adding 2 times of the mass of the absolute ethyl alcohol aqueous solution, stirring uniformly, standing for 12 hours, and taking supernatant;
step 3, adding 24 parts of the mixed percolate prepared in the step 1 into 36 parts of the supernatant in the step 2, stirring uniformly, standing for 24 hours, and taking the mixed supernatant for later use; adding 1 part of steviosin into 13 parts of the ginseng percolate prepared in the step 1, uniformly mixing, adding 3 parts of sodium benzoate, 0.3 part of ethylparaben and 50 parts of mixed supernatant, uniformly stirring, boiling, adding 20 parts of modified biochar under the boiling condition, performing centrifugal filtration at the centrifugal speed of 14000r/min for 10min, collecting the centrifugal liquid, filtering the centrifugal liquid by adopting a 0.45-micron nylon membrane, collecting filtrate, adding water to prepare 1000mL of solution, and uniformly stirring to obtain the Changchunbao oral liquid.
The preparation steps of the modified biochar in the step 3 are as follows, and the parts are all parts by weight:
s1, rinsing 20 parts of fructus forsythiae residues, 8 parts of corn straw residues and 15 parts of honeysuckle flower residues with water, and drying in a vacuum oven at 80 ℃ for 24 hours; then crushing by a grinder, sieving by a 100-mesh sieve, and collecting residue powder; carbonizing the residue powder at high temperature of 500 deg.C for 1h to obtain biochar;
s2, repeatedly washing 15 parts of the biochar prepared in the step S1 with water until the pH value of washing water is neutral, and drying in an oven at 80 ℃ for 24 hours to obtain dried biochar; mixing 10 parts of dry biochar, 15 parts of calcium chloride, 8 parts of ferric chloride, 4 parts of silicon dioxide and 80 parts of water, and stirring for 1 hour at constant temperature; and then grinding the dried solid, putting the ground solid into a tube furnace, heating the ground solid to 500 ℃ at the speed of 10 ℃/min, preserving the heat at 500 ℃ for 90min, rinsing the ground solid by using 200 parts of 0.1mol/L hydrochloric acid, washing the rinsed solid by using water until the pH value of a washing solution is neutral, drying the rinsed solid in an oven at 80 ℃ for 24h, grinding the rinsed solid, and sieving the ground solid by using a 100-mesh sieve to prepare the modified biochar.
Example 2
The preparation method of the Changchunbao oral liquid is basically the same as the example 1, and the only difference is that: the preparation method of the modified biochar in the step 3 is inconsistent.
The preparation steps of the modified biochar in the step 3 are as follows, and the parts are all parts by weight:
s1, rinsing 20 parts of fructus forsythiae residues, 8 parts of corn straw residues and 15 parts of honeysuckle flower residues with water, and drying in a vacuum oven at 80 ℃ for 24 hours; then crushing by a grinder, sieving by a 100-mesh sieve, and collecting residue powder; carbonizing the residue powder at high temperature of 500 deg.C for 1h to obtain biochar;
s2, repeatedly washing 15 parts of the biochar prepared in the step S1 with water until the pH value of washing water is neutral, and drying in an oven at 80 ℃ for 24 hours to obtain dried biochar; mixing 10 parts of dry biochar, 8 parts of ferric chloride, 4 parts of silicon dioxide and 80 parts of water, and stirring for 1 hour at constant temperature; and then grinding the dried solid, putting the ground solid into a tube furnace, heating the ground solid to 500 ℃ at the speed of 10 ℃/min, preserving the heat at 500 ℃ for 90min, rinsing the ground solid by 200 parts of 0.1mol/L hydrochloric acid, washing the rinsed solid by water until the pH value of a washing solution is neutral, drying the rinsed solid in an oven at 80 ℃ for 24h, grinding the rinsed solid, and sieving the ground solid by a 100-mesh sieve to prepare the modified biochar.
Example 3
The preparation method of the Changchunbao oral liquid is basically the same as the example 1, and the only difference is that: the preparation method of the modified biochar in the step 3 is inconsistent.
The preparation steps of the modified biochar in the step 3 are as follows, and the parts are all parts by weight:
s1, rinsing 20 parts of fructus forsythiae residues, 8 parts of corn straw residues and 15 parts of honeysuckle flower residues with water, and drying in a vacuum oven at 80 ℃ for 24 hours; then crushing by a grinder, sieving by a 100-mesh sieve, and collecting residue powder; carbonizing the residue powder at high temperature of 500 deg.C for 1h to obtain biochar;
s2, repeatedly washing 15 parts of biochar prepared by S1 with water until the pH value of washing water is neutral, and drying in an oven at 80 ℃ for 24 hours to obtain dried biochar; mixing 10 parts of dry biochar, 15 parts of calcium chloride, 4 parts of silicon dioxide and 80 parts of water, and stirring for 1 hour at constant temperature; and then grinding the dried solid, putting the ground solid into a tube furnace, heating the ground solid to 500 ℃ at the speed of 10 ℃/min, preserving the heat at 500 ℃ for 90min, rinsing the ground solid by 200 parts of 0.1mol/L hydrochloric acid, washing the rinsed solid by water until the pH value of a washing solution is neutral, drying the rinsed solid in an oven at 80 ℃ for 24h, grinding the rinsed solid, and sieving the ground solid by a 100-mesh sieve to prepare the modified biochar.
Example 4
The preparation method of the Changchunbao oral liquid is basically the same as the example 1, and the only difference is that: the preparation method of the modified biochar in the step 3 is inconsistent.
The preparation steps of the modified biochar in the step 3 are as follows, and the parts are all parts by weight:
s1, rinsing 20 parts of fructus forsythiae residues, 8 parts of corn straw residues and 15 parts of honeysuckle flower residues with water, and drying in a vacuum oven at 80 ℃ for 24 hours; then crushing by a grinder, sieving by a 100-mesh sieve, and collecting residue powder; carbonizing the residue powder at high temperature of 500 deg.C for 1h to obtain biochar;
s2, repeatedly washing 15 parts of biochar prepared by S1 with water until the pH value of washing water is neutral, and drying in an oven at 80 ℃ for 24 hours to obtain dried biochar; mixing 10 parts of dry biochar, 15 parts of calcium chloride, 8 parts of ferric chloride and 80 parts of water, and stirring for 1 hour at constant temperature; and then grinding the dried solid, putting the ground solid into a tube furnace, heating the ground solid to 500 ℃ at the speed of 10 ℃/min, preserving the heat at 500 ℃ for 90min, rinsing the ground solid by using 200 parts of 0.1mol/L hydrochloric acid, washing the rinsed solid by using water until the pH value of a washing solution is neutral, drying the washed solid in an oven at 80 ℃ for 24h, grinding the washed solid, and sieving the ground solid by using a 100-mesh sieve to prepare the modified biochar.
Comparative example 1
The preparation method of the Changchunbao oral liquid is basically the same as the example 1, and the only difference is that: and replacing the modified biochar in the step 3 with biochar.
The preparation steps of the biochar in the step 3 are as follows, and the biochar is prepared from the following raw materials in parts by weight:
s1, rinsing 20 parts of fructus forsythiae residues, 8 parts of corn straw residues and 15 parts of honeysuckle flower residues with water, and drying in a vacuum oven at 80 ℃ for 24 hours; then crushing by a grinder, sieving by a 100-mesh sieve, and collecting residue powder; carbonizing the residue powder at a limited oxygen control temperature of 500 ℃ for 1h to obtain biochar;
comparative example 2
The preparation method of the Changchunbao oral liquid is basically the same as the example 1, and the only difference is that: modified biochar is not added in the step 3.
Test example 1
Anti-allergic Performance test
The test method refers to doctor thesis (research on dangerous factors causing anaphylactic reaction of traditional Chinese medicines and allergic components of Chinese patent medicines, author: Linmingbao, Zhejiang university, 2013), animal quality and source: BALB/c mice, clean grade, 70 mice, weight 18-22 g, female, provided by institutional animals institute of Tongji medical college, university of science and technology, Huazhong. The test method is as follows:
1. setting a blank control group, randomly dividing the mice into 7 groups of 10 mice, feeding the blank control group with standard feed of experimental mice once a day, wherein the feed is 6g each time, and simultaneously feeding 5mL of distilled water; examples and comparative mice were fed with the same feed once a day, 6g per feed, while feeding 3mL of distilled water and 2mL of vinpocetine oral liquid.
2. Feeding in environment with temperature of 23 + -3 deg.C, relative temperature of 50 + -5 deg.C, artificial illumination for 12 hr and ventilation for 12 times/hr for 90 days. After feeding, blood is taken from orbital veins of the mice and is frozen for standby; after blood collection, the mice are placed in 75 wt% ethanol water solution to be soaked for 1min, popliteal lymph nodes on two back sides of the mice are picked up in an ultra-static workbench, the popliteal lymph nodes are placed in 1 wt% BSAPBS, peripheral adipose tissues are carefully separated and removed, and the mice are weighed in a ten-thousandth analytical balance by a weight loss method. PLN lymph node indices and cell counts were performed. The average values of the multiple tests are shown in Table 1. Another mouse liver tissue was frozen with liquid nitrogen and stored for liver function test in test example 2.
TABLE 1 anti-allergic Performance test in mice
Figure BDA0003286373130000111
As can be seen from the test results in table 1, the mouse in example 1 has the lowest lymphocyte index and the lowest lymphocyte number in 90 days of feeding, which may be caused by selecting the residues of forsythia, corn stalks and honeysuckle as the source of biochar, the biochar prepared from the residues has a developed pore structure, and the biochar has a strong adsorption capacity due to the abundant open pores and functional groups on the surface, so that the content of allergens in the Chinese herbal medicines can be reduced, and the adsorption capacity is improved by modifying with calcium chloride, ferric chloride and silicon dioxide. The specific surface area of the modified biochar is greatly increased, calcium, iron and chloride ions are attached to the biochar, and oxygen-containing functional groups on the allergic molecules can be combined with the biochar surface through hydrogen bonds. The functional groups such as hydroxyl, amine and the like in the allergen can be combined with metal cations on the biochar, so that the adsorption of allergen components is enhanced.
Test example 2
Liver function test in mice
The blood and liver collected in test example 1 were subjected to liver function test using alanine Aminotransferase (ALT), aspartate Aminotransferase (AST), and alkaline phosphatase (ALP). The average values of the multiple tests are shown in Table 2.
TABLE 2 liver function test table for mice
Figure BDA0003286373130000121
When severe necrosis or destruction of the liver occurs, alanine Aminotransferase (ALT), aspartate Aminotransferase (AST), and alkaline phosphatase (ALP) are present in high serum concentrations. The three enzymes are widely distributed in tissues such as human liver, bone, intestine, kidney, placenta and the like and are discharged outwards through the liver, and can be used as indexes for detecting diseases such as obstructive yellow pox, primary liver cancer, secondary liver cancer, bile migration hepatitis and the like, and the determination results in a table 2 show that the liver functions of the example 1 and the blank control group are normal, and the phenomena such as oxidative phosphorylation of the functions of liver cell mitochondria, liver cell edema, fatty degeneration, partial necrosis and the like are probably caused by taking the traditional Chinese medicine containing the polygonum multiflorum for a long time, wherein the traditional Chinese medicine contains anthraquinone compounds (particularly emodin and derivatives thereof); the residues of fructus forsythiae, corn stalks and honeysuckle flowers are selected as the source of the biochar, the biochar prepared from the residues has a developed pore structure, calcium chloride, ferric chloride and silicon dioxide are further adopted for modification, and the modified biochar has a large specific surface areaThe calcium, iron and chloride ions are attached to the biochar. Ca2+The existence of the active carbon neutralizes anions on the surface of the biochar, reduces electrostatic repulsion, and is constructed into a microporous adsorbent, oxygen-containing functional groups on molecules of anthraquinone toxic components can be combined with the surface of the biochar through hydrogen bonds, so that the Changchun Bao oral liquid adsorbed by the modified active carbon hardly contains the anthraquinone toxic components which hurt the liver.
Test example 3
Memory performance testing
The pH value, moisture content and content of the Changchunbao oral liquid are measured by visual inspection and systematic measurement in the examples and the comparative examples. The storage conditions are 25 ℃ plus or minus 2 ℃ and the humidity is 60 ℃ plus or minus 5%, the detection results show that the prepared Changchun bao oral liquid is light black liquid within 6 months, the clarity and the color of the solution are not obviously changed, the filling quantity difference, visible foreign matters and insoluble particles all accord with the regulations, the pH value and the moisture of the Changchun bao oral liquid are measured after the preparation and the storage for 6 months, the average value is obtained through multiple tests, and the detection results are shown in Table 3.
TABLE 3 results of the storage property test of Changchunbao oral liquid
Figure BDA0003286373130000131
As can be seen from Table 3, the change in pH and moisture in example 1 was minimized, probably because the filtration effect of the modified activated carbon removed unstable components such as hydroxyl and carboxyl groups in the oral liquid, thereby preventing deterioration and hydrolysis during the later storage and prolonging the storage time of the oral liquid.

Claims (9)

1. The preparation method of the oral liquid is characterized by comprising the following steps:
step 1, grinding ginseng, rhizoma alismatis, prepared polygonum multiflorum, angelica sinensis, schisandra chinensis and eucommia ulmoides respectively, and sieving the ground materials by adopting a 50-200-mesh sieve; then, soaking the ginseng powder by using 20-40 wt% of ethanol water solution as a solvent and 60-80 wt% of ethanol water solution as a solvent after mixing the alisma orientale powder, the prepared polygonum multiflorum powder, the angelica powder, the schisandra chinensis powder and the eucommia ulmoides powder for 5-20 hours, percolating, wherein the outflow rate of percolate is 1-3 mL/min, collecting percolate, and preparing adult ginseng percolate and mixed percolate;
step 2, adding water into rhizoma anemarrhenae, cortex phellodendri, fructus lycii, Chinese yam, radix asparagi, fructus psoraleae, rhizoma curculiginis, parasitic loranthus, radix ophiopogonis, glossy privet fruit, rehmannia glutinosa, herba ecliptae, prepared rehmannia root, radix achyranthis bidentatae, radix salviae miltiorrhizae, poria cocos, morinda officinalis, herba epimedii and radix astragali, decocting for two times, adding water for the first time, decocting for 1-3 hours, collecting decoction, adding water for the second time, decocting for 1-3 hours, and collecting decoction; mixing the two decoctions, filtering by using a filter screen of 50-200 meshes, then evaporating and concentrating until the relative density is 1.06-1.09 at 65 ℃, the evaporation temperature is 60-70 ℃, adding 1-3 times of absolute ethyl alcohol by mass, stirring uniformly, standing for 5-15 h, and taking supernatant;
step 3, adding the mixed percolate prepared in the step 1 into the supernatant obtained in the step 2, stirring uniformly, standing for 10-30 h, and taking the mixed supernatant for later use; and adding stevioside into the ginseng percolate prepared in the step 1, uniformly mixing, adding sodium benzoate, ethylparaben and mixed supernatant, uniformly stirring, boiling, adding modified biochar under the boiling condition, performing centrifugal filtration at the centrifugal speed of 12000-15000 r/min for 5-20 min, collecting the centrifugal liquid, filtering the centrifugal liquid by using a 0.1-1 mu m nylon membrane, collecting filtrate, adding water to prepare 500-1500 mL of solution, and uniformly stirring to obtain the periwinkle oral liquid.
2. The method for preparing oral liquid according to claim 1, wherein the components in the step 1 are calculated by weight parts: 10-20 parts of ginseng, 20-30 parts of rhizoma alismatis, 20-30 parts of prepared polygonum multiflorum, 12-20 parts of angelica sinensis, 5-12 parts of schisandra chinensis, 8-15 parts of eucommia ulmoides, 50-150 parts of 20-40 wt% ethanol water solution and 300-500 parts of 60-80 wt% ethanol water solution.
3. The method for preparing an oral liquid according to claim 1, wherein: the percolation method adopted in the step 1 is one of a single percolation method, a double percolation method, a pressure percolation method and a counter-current percolation method.
4. The method for preparing oral liquid according to claim 1, wherein the components in the step 2 are calculated by weight parts: 8-15 parts of rhizoma anemarrhenae, 8-15 parts of cortex phellodendri, 10-20 parts of fructus lycii, 5-15 parts of Chinese yam, 10-20 parts of radix asparagi, 10-20 parts of fructus psoraleae, 5-12 parts of rhizoma curculiginis, 10-20 parts of parasitic loranthus, 10-20 parts of radix ophiopogonis, 15-25 parts of glossy privet fruit, 10-20 parts of rehmannia, 15-25 parts of herba ecliptae, 10-20 parts of prepared rehmannia root, 10-20 parts of radix achyranthis bidentatae, 10-20 parts of radix salviae miltiorrhizae, 10-20 parts of poria cocos, 10-20 parts of radix morindae officinalis, 5-12 parts of herba epimedii, 10-20 parts of radix astragali, 1400-2000 parts of water for the first time and 1000-1500 parts of water for the second time.
5. The method for preparing oral liquid according to claim 1, wherein the components in the step 3 are calculated by weight parts: 30-50 parts of the supernatant in the step 2, 20-30 parts of the mixed percolate prepared in the step 1, 0.5-2 parts of steviosin, 10-20 parts of the ginseng percolate prepared in the step 1, 1-5 parts of sodium benzoate, 0.1-0.5 part of ethylparaben, 40-60 parts of the mixed supernatant and 10-30 parts of modified biochar.
6. The method for preparing oral liquid according to claim 1, wherein the modified biochar in the step 3 is prepared by the following steps:
s1, rinsing the fructus forsythiae residues, the corn straw residues and the honeysuckle residues with water, and drying at 70-90 ℃ for 10-30 hours; then crushing, sieving by using a 50-200 mesh sieve, and collecting residue powder; carbonizing the residue powder at a high temperature of 400-600 ℃ for 0.5-2 h to obtain biochar;
s2, repeatedly washing the biochar prepared in the step S1 with water until the pH value of the washing water is neutral, and drying the biochar in an oven at 70-90 ℃ for 20-30 hours to obtain dried biochar; adding calcium chloride, ferric chloride, silicon dioxide and water into the dried biochar, mixing, and stirring for 0.5-2 h; and then putting the mixture into a high-temperature environment, heating the mixture to 400-600 ℃ at a speed of 5-15 ℃/min, preserving the heat at 400-600 ℃ for 50-150 min, rinsing the mixture by using 0.01-0.5 mol/L hydrochloric acid, washing the rinsed mixture by using water until the pH value of a washing solution is neutral, drying the rinsed mixture for 10-30 h at 70-90 ℃, grinding the rinsed mixture, and sieving the ground mixture by using a 50-200-mesh sieve to prepare the modified biochar.
7. The method for preparing an oral liquid according to claim 6, wherein the components in the step S1 are calculated by weight parts: 10-30 parts of fructus forsythiae residues, 5-15 parts of corn straw residues and 10-20 parts of honeysuckle flower residues.
8. The method for preparing an oral liquid according to claim 6, wherein the components in the step S2 are calculated by weight parts: 10-20 parts of the biochar prepared in the step S1, 5-15 parts of dried biochar, 10-20 parts of calcium chloride, 5-15 parts of ferric chloride, 1-6 parts of silicon dioxide, 70-100 parts of water and 100-300 parts of 0.01-0.5 mol/L hydrochloric acid.
9. An oral liquid, which is characterized in that: the preparation method of the oral liquid is used for preparing the oral liquid as claimed in any one of claims 1 to 8.
CN202111149361.9A 2021-09-29 2021-09-29 Oral liquid and preparation method thereof Pending CN113908227A (en)

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