CN113616725A - Preparation method of Danting Lung-Heart granules - Google Patents
Preparation method of Danting Lung-Heart granules Download PDFInfo
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- CN113616725A CN113616725A CN202111056241.4A CN202111056241A CN113616725A CN 113616725 A CN113616725 A CN 113616725A CN 202111056241 A CN202111056241 A CN 202111056241A CN 113616725 A CN113616725 A CN 113616725A
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Abstract
The preparation method of the danting pulmonary heart granules comprises the following steps: (1) taking fructus aurantii, bitter almond, whiteflower hogfennel root, szechuan lovage rhizome, salvia miltiorrhiza, 1/2 parts of thunberg fritillary bulb and heartleaf houttuynia herb, crushing, adding into a high-pressure reaction kettle, adding warm water and 0.1-0.3% of cellulase, uniformly stirring, reacting for 5-8min under the pressure of 0.3-0.5 MPa and the pH value of 4.5-5.5; (2) taking cortex mori radicis, liquorice, radix pseudostellariae, semen lepidii and gypsum, crushing, adding into a high-pressure reaction kettle, adding absolute ethyl alcohol and 0.1-0.3% of cellulase, uniformly stirring under the pressure of 0.2-0.3 MPa and the pH value of 4.5-5.5, and reacting for 3-5 min; (3) extracting the medicinal materials in the step (1) and the honey ephedra by 95 percent ethanol at normal temperature and high pressure; (4) decocting the medicinal materials in the step (2) in water; (5) mixing the concentrated solution of step (3) and the supernatant concentrated solution obtained by decocting the concentrated solution of step (4) with water, precipitating with ethanol, and concentrating to obtain fluid extract; (6) mixing the fluid extract, adjuvants and the rest fine powder of Bulbus Fritillariae Thunbergii, stirring, and making into granule. The method has short production period and low energy consumption, can extract effective components from medicinal materials to the maximum extent, and has better therapeutic effect than the conventional method.
Description
Technical Field
The invention relates to the field of preparation methods of traditional Chinese medicine preparations, in particular to a preparation method of Dan Ting Fei Xin granules.
Background
The Dantingfeixianxin granules are a traditional Chinese medicine preparation (application number: 200310110028.2) which is processed by mix-fried ephedra herb, gypsum, heartleaf houttuynia herb, whiteflower hogfennel root, bitter apricot seed, thunberg fritillary bulb, pepperweed seed, white mulberry root-bark, bitter orange, danshen root, Szechuan lovage rhizome, heterophylly falsestarwort root, liquoric root and auxiliary materials; has the effects of clearing heat, eliminating phlegm, relieving cough and asthma, and is used for treating pulmonary heart disease (attack stage) which belongs to phlegm-heat syndrome, and the syndrome is shown as follows: cough, dyspnea, yellow and sticky sputum, or chest distress, palpitation, fever, cyanosis of lips, dry stool, red tongue with yellow or greasy coating, etc. The traditional process for preparing the danting pulmonary heart granules comprises the following steps: (1) reflux-extracting fructus Aurantii, semen Armeniacae amarum, herba Ephedrae preparata, radix Peucedani, rhizoma Ligustici Chuanxiong, Saviae Miltiorrhizae radix, and Bulbus Fritillariae Thunbergii 1/2 with 70-80% ethanol for three times, filtering, mixing filtrates, recovering ethanol under reduced pressure, and collecting medicinal liquid; (2) decocting the dregs of the step (1) and the other six medicines together with water twice, filtering, combining the filtrates, concentrating the filtrate, precipitating with ethanol, and concentrating the supernatant; (3) mixing the liquid medicines in the step (1) and the step (2), and concentrating to obtain clear paste; (4) pulverizing the rest 1/2 amount of Bulbus Fritillariae Thunbergii into fine powder, mixing fluid extract, sucrose, dextrin and Bulbus Fritillariae Thunbergii fine powder, stirring, granulating, drying at low temperature, and grading. The preparation method has long production period, needs about 10 days to finish the final whole grain from extraction, and has the advantages of repeated heating in the whole extraction process, high energy consumption and high production cost.
Disclosure of Invention
The invention aims to provide a preparation method of Dandelion pulmonary heart granules, which has the advantages of short production period and low energy consumption, can extract effective components in medicinal materials to the maximum extent, and has better treatment effect than the Dandelion pulmonary heart granules prepared by the traditional method.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the danting pulmonary heart granules comprises the following steps:
s1, taking bitter orange, bitter apricot seed, whiteflower hogfennel root, Szechuan lovage rhizome, red sage root, 1/2 amount of thunberg fritillary bulb and heartleaf houttuynia herb, crushing the bitter orange, the bitter apricot seed, the whiteflower hogfennel root, the Szechuan lovage rhizome, the red sage root, the 1/2 amount of thunberg fritillary bulb and the heartleaf houttuynia herb into blocky particles with the size of 0.5-1cm, adding the blocky particles into a high-pressure reaction kettle, adding warm water with the temperature of 35-40 ℃ and cellulase with the weight of 0.1-0.3% of the medicinal materials into the high-pressure reaction kettle, uniformly stirring, controlling the pressure to be 0.3-0.5 MPa and the PH to be 4.5-5.5, and reacting for 5-8 min;
step S2, taking cortex mori radicis, liquorice, radix pseudostellariae, semen lepidii and gypsum, crushing the cortex mori radicis, the liquorice, the radix pseudostellariae, the semen lepidii and the gypsum into 0.5-1 cm-sized blocky particles, adding the blocky particles into a high-pressure reaction kettle, adding anhydrous ethanol with the temperature of 40-45 ℃ and cellulase with the weight of 0.1-0.3% of the medicinal materials into the high-pressure reaction kettle, stirring and uniformly mixing the materials, controlling the pressure to be 0.2-0.3 MPa and the PH to be 4.5-5.5, and reacting for 3-5 min;
s3, taking out the medicinal materials in the step S1, washing with warm water, draining, putting the medicinal materials and the crushed Chinese ephedra into a high-pressure device, adding 95% ethanol, extracting at normal temperature, controlling the pressure to be 103-115 MPa, extracting for 10-20min, filtering, concentrating the ethanol extract, and keeping dregs for later use;
s4, taking out the medicinal materials in the step S2, washing with warm water, draining, putting the medicinal materials and the dregs in the step S3 into water, decocting for 40-60min, filtering, concentrating the water extract, adding ethanol under ice bath until the alcohol content reaches 75%, stirring uniformly, standing for 8 hours, filtering to obtain a supernatant, and recovering the ethanol under reduced pressure;
step S5, mixing the ethanol extraction concentrated solution in the step 3 with the supernatant concentrated solution in the step S4, and concentrating to obtain clear paste;
step S6, grinding the rest 1/2 amount of thunberg fritillary bulb into fine powder, then taking the clear paste of the step S5, auxiliary materials and the fine powder of the thunberg fritillary bulb, stirring evenly, and preparing into granules.
Preferably, in the step S1, the amount of the warm water is 2-3cm higher than that of the medicinal materials after all the medicinal materials are soaked; the amount of the absolute ethyl alcohol in the step S2 is 2-3cm after all the medicinal materials are soaked.
Preferably, the medicinal material in the step S1 is crushed, then is put into an oven to be baked to 35-40 ℃, and then is added into a high-pressure reaction kettle; the medicinal material in the step S2 is crushed, then is put into an oven to be baked to 40-45 ℃, and then is added into a high-pressure reaction kettle.
Preferably, in step S4, after the ethanol precipitation filtration, the precipitate is washed once with 75% ethanol, filtered, and the washing solution and the supernatant are combined, and then the ethanol is recovered under reduced pressure.
The invention has the advantages and beneficial effects that:
(1) according to the preparation method provided by the invention, the medicinal materials are treated by the cellulase before ethanol high-pressure extraction and water decoction, the cell walls of the medicinal materials are changed to different degrees by reasonably controlling the amount of the cellulase and the reaction temperature and time, and meanwhile, the effective components in the medicinal materials are prevented from being lost, so that the time for subsequent ethanol extraction and water decoction is shortened, and the extraction rate is improved.
(2) The preparation method provided by the invention adopts high-pressure extraction during ethanol extraction, and the high-pressure extraction can fully extract the components in the medicinal materials in a short time, thereby shortening the extraction time and further improving the extraction efficiency; meanwhile, the high-pressure extraction is carried out at normal temperature, so that partial components in the medicinal materials can be prevented from losing activity, and the treatment effect of the medicament is improved.
(3) The preparation method provided by the invention changes the traditional preparation mode, the traditional Chinese medicines such as the houttuynia cordata, the bitter orange, the bitter apricot seed and the like are firstly extracted by alcohol, and then the decoction dregs are decocted by water, so that the adjustment mode can greatly provide the treatment effect of the medicines.
(4) The preparation method provided by the invention has the advantages that the ethanol extraction and the water decoction extraction are carried out once, the production period is short, and the preparation method can shorten half the time compared with the traditional preparation method; in addition, 95% ethanol is adopted for extraction at normal temperature and high pressure during ethanol extraction, so that the effective components in the medicinal materials can be extracted to the maximum extent, and all steps and improvement of process parameters are integrated, so that the finally prepared Dandeli lung-heart granules have obviously better treatment effect than the Dandeli lung-heart granules prepared by the traditional method.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The preparation method of the danting pulmonary heart granules comprises the following steps:
step S1, taking 9 parts by weight of fructus Aurantii, 9 parts by weight of semen Armeniacae amarum, 12 parts by weight of radix Peucedani, 6 parts by weight of rhizoma Ligustici Chuanxiong, 9 parts by weight of Saviae Miltiorrhizae radix, 6 parts by weight of Bulbus Fritillariae Thunbergii and 15 parts by weight of herba Houttuyniae, pulverizing into 0.5-1cm block-shaped particles, and baking in oven to medicinal material temperature of 35-40 deg.C; then adding the baked medicinal materials into a high-pressure reaction kettle, adding warm water with the temperature of 35-40 ℃ and cellulase accounting for 0.2% of the weight of the medicinal materials into the high-pressure reaction kettle, wherein the amount of the warm water is 2-3cm higher than that of the medicinal materials after all the medicinal materials are soaked, uniformly stirring, controlling the pressure to be 0.3-0.5 MPa and the pH to be 4.5-5.5, and reacting for 5-8 min;
step S2, taking 12 parts by weight of white mulberry root-bark, 6 parts by weight of liquorice, 10 parts by weight of radix pseudostellariae, 12 parts by weight of semen lepidii and 18 parts by weight of gypsum, crushing the materials into 0.5-1 cm-sized blocky particles, and then baking the blocky particles in an oven until the temperature of the medicinal materials is 40-45 ℃; adding the baked medicinal materials into a high-pressure reaction kettle, adding 40-45 ℃ absolute ethyl alcohol and 0.2% cellulase by weight of the medicinal materials into the high-pressure reaction kettle, stirring and uniformly mixing the absolute ethyl alcohol with the amount of 2-3cm higher than that of the medicinal materials after all the medicinal materials are soaked, controlling the pressure to be 0.2-0.3 MPa and the PH to be 4.5-5.5, and reacting for 3-5 min;
s3, taking out the medicinal materials in the step S1, washing with warm water, draining (no water dripping), putting the medicinal materials and the crushed Chinese ephedra (6 parts by weight) into a high-pressure device, adding 95% ethanol, extracting at normal temperature for 10-20min under the pressure of 103-115 MPa, filtering, concentrating the ethanol extract, and keeping dregs for later use;
s4, taking out the medicinal materials in the step S2, washing with warm water, draining (no water dripping is needed), putting the medicinal materials and the dregs in the step S3 into water, decocting for 40-60min, filtering, concentrating the water extract until the relative density is about 1.13-1.16(50 ℃), adding ethanol under ice bath until the alcohol content reaches 75%, stirring uniformly, standing for 8 hours, filtering to obtain supernatant, stirring and washing the precipitate with 75% ethanol once, filtering, combining the washing liquid and the supernatant, and recovering the ethanol under reduced pressure;
step S5, mixing the concentrated solution in step S3 with the concentrated solution in step S4, and concentrating to obtain fluid extract (the relative density is 1.28-1.30 measured at 80 deg.C);
step S6, grinding the rest 6 weight parts of thunberg fritillary bulb into fine powder (100 meshes), then taking 1 weight part of clear paste of the step S5, 3 weight parts of cane sugar, 0.5 weight part of dextrin and the fine powder of the thunberg fritillary bulb, stirring uniformly, preparing into granules, drying at low temperature (60 ℃), finishing granules and subpackaging.
Example 2
The preparation method of the danting pulmonary heart granules comprises the following steps:
step S1, taking 9 parts by weight of fructus Aurantii, 9 parts by weight of semen Armeniacae amarum, 12 parts by weight of radix Peucedani, 6 parts by weight of rhizoma Ligustici Chuanxiong, 9 parts by weight of Saviae Miltiorrhizae radix, 6 parts by weight of Bulbus Fritillariae Thunbergii and 15 parts by weight of herba Houttuyniae, pulverizing into 0.5-1cm block-shaped particles, and baking in oven to medicinal material temperature of 35-40 deg.C; then adding the baked medicinal materials into a high-pressure reaction kettle, adding warm water with the temperature of 35-40 ℃ and cellulase accounting for 0.1% of the weight of the medicinal materials into the high-pressure reaction kettle, wherein the amount of the warm water is 2-3cm higher than that of the medicinal materials after all the medicinal materials are soaked, uniformly stirring, controlling the pressure to be 0.3-0.5 MPa and the pH to be 4.5-5.5, and reacting for 5-8 min;
step S2, taking 12 parts by weight of white mulberry root-bark, 6 parts by weight of liquorice, 10 parts by weight of radix pseudostellariae, 12 parts by weight of semen lepidii and 18 parts by weight of gypsum, crushing the materials into 0.5-1 cm-sized blocky particles, and then baking the blocky particles in an oven until the temperature of the medicinal materials is 40-45 ℃; adding the baked medicinal materials into a high-pressure reaction kettle, adding 40-45 ℃ absolute ethyl alcohol and cellulase accounting for 0.3 percent of the weight of the medicinal materials into the high-pressure reaction kettle, stirring and uniformly mixing the absolute ethyl alcohol with the amount of 2-3cm higher than that of the medicinal materials after all the medicinal materials are soaked, controlling the pressure to be 0.2-0.3 MPa and the PH to be 4.5-5.5, and reacting for 3-5 min;
s3, taking out the medicinal materials in the step S1, washing with warm water, draining (no water dripping), putting the medicinal materials and the crushed Chinese ephedra (6 parts by weight) into a high-pressure device, adding 95% ethanol, extracting at normal temperature for 10-20min under the pressure of 103-115 MPa, filtering, concentrating the ethanol extract, and keeping dregs for later use;
s4, taking out the medicinal materials in the step S2, washing with warm water, draining (no water dripping is needed), putting the medicinal materials and the dregs in the step S3 into water, decocting for 40-60min, filtering, concentrating the water extract until the relative density is about 1.13-1.16(50 ℃), adding ethanol under ice bath until the alcohol content reaches 75%, stirring uniformly, standing for 8 hours, filtering to obtain supernatant, stirring and washing the precipitate with 75% ethanol once, filtering, combining the washing liquid and the supernatant, and recovering the ethanol under reduced pressure;
step S5, mixing the concentrated solution obtained in step S3 and the concentrated solution obtained in step S4, and concentrating to obtain fluid extract (the relative density is 1.28-1.30 measured at 80 ℃);
step S6, grinding the rest 6 weight parts of thunberg fritillary bulb into fine powder (100 meshes), then taking 1 weight part of clear paste of the step S5, 3 weight parts of cane sugar, 0.5 weight part of dextrin and the fine powder of the thunberg fritillary bulb, stirring uniformly, preparing into granules, drying at low temperature (60 ℃), finishing granules and subpackaging.
Comparative example 1
The preparation method of the danting pulmonary heart granules comprises the following steps:
step S1, taking 9 parts by weight of fructus Aurantii, 9 parts by weight of semen Armeniacae amarum, 6 parts by weight of herba Ephedrae preparata (herba Ephedrae honey), 12 parts by weight of radix Peucedani, 6 parts by weight of rhizoma Ligustici Chuanxiong, 9 parts by weight of Saviae Miltiorrhizae radix, and 1/2 parts by weight of Bulbus Fritillariae Thunbergii (6 parts by weight), extracting with 80% ethanol under reflux for three times (2 hr, 1.5 hr), filtering, mixing filtrates, recovering ethanol under reduced pressure, and collecting medicinal liquid;
step S2, decocting the residue obtained in step S1 and the rest six medicines (15 parts by weight of houttuynia cordata, 12 parts by weight of cortex mori radicis, 6 parts by weight of liquorice, 10 parts by weight of radix pseudostellariae, 12 parts by weight of semen lepidii and 18 parts by weight of gypsum) in water for two times (2 hours and 2 hours), filtering, merging the filtrate, concentrating the filtrate, precipitating with ethanol (the ethanol is added to ensure that the content is 60 percent, stirring uniformly, standing for 12 hours), filtering to obtain supernatant, stirring and washing the precipitate with 60 percent ethanol once, filtering, merging the washing liquor and the supernatant, and recovering the ethanol under reduced pressure;
step S3, merging the liquid medicines in the step S1 and the step S2, and concentrating to obtain clear paste;
step S4, grinding the rest 1/2 amount of thunberg fritillary bulb into fine powder (100 meshes), taking 1 weight part of clear paste, 3 weight parts of cane sugar, 0.5 weight part of dextrin and the fine powder of the thunberg fritillary bulb, stirring uniformly, preparing into granules, drying at low temperature (60 ℃), finishing granules and subpackaging.
Need to explain: in the invention, various improved schemes are tried when the preparation method is determined, and because the traditional Chinese medicinal materials are mixed and subjected to high-pressure ethanol extraction and water decoction, a great amount of tests are also carried out on selection of specific process parameters in each step, and finally the method provided by the invention is determined to have the best effect. In order to highlight the focus of the present invention, the failed schemes are not illustrated in the present invention.
Clinical experiments
1. Data and method
1.1, study object
According to the invention, 64 patients diagnosed with the pulmonary heart disease are taken as research objects, the patients know the information and agree to participate in clinical tests, and the patients are all in accordance with the diagnosis of the chronic pulmonary heart disease and have no other induced diseases. Randomly dividing 60 patients into 2 groups, wherein the ages of the patients in the conventional group are 45-60 years old, 14 patients in male patients and 18 patients in female patients; the patients in the test group are 45-65 years old, 16 male patients and 16 female patients, and the general data of the patients do not have statistical difference.
1.2 methods of treatment
The pellet prepared in the comparative example 1 is taken with warm water 10g each time and 3 times a day for 4 weeks in a conventional group; the test group was administered with the pellet of Danting Lung Heart prepared in example 1, 10g each time, 3 times a day, continuously for 4 weeks, with warm boiled water.
1.3, observation index
The heart function of the patient after treatment is investigated, and the treatment effect of the patient is evaluated according to the heart function of the patient. And meanwhile, the occurrence condition of adverse reaction in the treatment process of the patient is observed.
1.4 evaluation index
Remarkably: the cardiac function of the patient is improved by more than grade 2 after treatment, or the cardiac function of the patient reaches grade I.
The improvement is as follows: the patients had improved cardiac function beyond grade 1 but did not reach grade i after treatment.
And (4) invalidation: the patients have no improvement or even aggravation after treatment.
The effective rate is (significant number + improved number)/total number.
1.5 statistical analysis
Data were processed using the sps 20.0 software, and data in% counts. P < 0.05 considered the difference to be statistically significant.
2. Results
2.1 comparison of therapeutic effects
The effective rate of the curative effect evaluation of the patients in the test group is 96.88%, and the significant efficiency is 56.25%; the effective rate of the conventional group is 87.50 percent, and the significant efficiency is 37.50 percent; p is less than 0.05, and is detailed in Table 1.
2.2 adverse reactions
The patients in the conventional group and the experimental group have no adverse reaction in the treatment process.
TABLE 1 therapeutic effect comparison table
Claims (4)
1. The preparation method of the danting pulmonary heart granules is characterized by comprising the following steps:
s1, taking bitter orange, bitter apricot seed, whiteflower hogfennel root, Szechuan lovage rhizome, red sage root, 1/2 amount of thunberg fritillary bulb and heartleaf houttuynia herb, crushing the bitter orange, the bitter apricot seed, the whiteflower hogfennel root, the Szechuan lovage rhizome, the red sage root, the 1/2 amount of thunberg fritillary bulb and the heartleaf houttuynia herb into blocky particles with the size of 0.5-1cm, adding the blocky particles into a high-pressure reaction kettle, adding warm water with the temperature of 35-40 ℃ and cellulase with the weight of 0.1-0.3% of the medicinal materials into the high-pressure reaction kettle, uniformly stirring, controlling the pressure to be 0.3-0.5 MPa and the PH to be 4.5-5.5, and reacting for 5-8 min;
step S2, taking cortex mori radicis, liquorice, radix pseudostellariae, semen lepidii and gypsum, crushing the cortex mori radicis, the liquorice, the radix pseudostellariae, the semen lepidii and the gypsum into 0.5-1 cm-sized blocky particles, adding the blocky particles into a high-pressure reaction kettle, adding anhydrous ethanol with the temperature of 40-45 ℃ and cellulase with the weight of 0.1-0.3% of the medicinal materials into the high-pressure reaction kettle, stirring and uniformly mixing the materials, controlling the pressure to be 0.2-0.3 MPa and the PH to be 4.5-5.5, and reacting for 3-5 min;
s3, taking out the medicinal materials in the step S1, washing with warm water, draining, putting the medicinal materials and the crushed Chinese ephedra into a high-pressure device, adding 95% ethanol, extracting at normal temperature, controlling the pressure to be 103-115 MPa, extracting for 10-20min, filtering, concentrating the ethanol extract, and keeping dregs for later use;
s4, taking out the medicinal materials in the step S2, washing with warm water, draining, putting the medicinal materials and the dregs in the step S3 into water, decocting for 40-60min, filtering, concentrating the water extract, adding ethanol under ice bath until the alcohol content reaches 75%, stirring uniformly, standing for 8 hours, filtering to obtain a supernatant, and recovering the ethanol under reduced pressure;
step S5, mixing the ethanol extraction concentrated solution obtained in the step S3 with the supernatant concentrated solution obtained in the step S4, and concentrating to obtain clear paste;
step S6, grinding the rest 1/2 amount of thunberg fritillary bulb into fine powder, then taking the clear paste of the step S5, auxiliary materials and the fine powder of the thunberg fritillary bulb, stirring evenly, and preparing into granules.
2. The method for preparing the danting feixuan granule according to claim 1, wherein the amount of the warm water in the step S1 is 2-3cm higher than that of the medicinal materials after all the medicinal materials are soaked; the amount of the absolute ethyl alcohol in the step S2 is 2-3cm after all the medicinal materials are soaked.
3. The method for preparing the danting feixuan granules according to claim 1, wherein the medicinal material of the step S1 is crushed, baked in an oven to 35-40 ℃ and then added into a high-pressure reaction kettle; the medicinal material in the step S2 is crushed, then is put into an oven to be baked to 40-45 ℃, and then is added into a high-pressure reaction kettle.
4. The method for preparing the danting feixuan granule according to claim 1, wherein the precipitate after the alcohol precipitation filtration in the step S4 is washed with 75% ethanol by stirring once, filtered, and the washing solution and the supernatant are combined, and then the ethanol is recovered under reduced pressure.
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CN111494271A (en) * | 2020-06-19 | 2020-08-07 | 广州智尚生物科技有限公司 | Atractylodes lancea rhizome and hypericum perforatum mixed extract and preparation method and application thereof |
CN112439025A (en) * | 2020-12-16 | 2021-03-05 | 江西和明制药有限公司 | Preparation method of Maiwei rehmannia oral liquid |
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CN1544022A (en) * | 2003-11-14 | 2004-11-10 | 玉 王 | Chinese traditional medicine particle for treating pulmonary heart disease |
CN106434076A (en) * | 2016-09-05 | 2017-02-22 | 广西大学 | Rambutan shell beer |
CN111494271A (en) * | 2020-06-19 | 2020-08-07 | 广州智尚生物科技有限公司 | Atractylodes lancea rhizome and hypericum perforatum mixed extract and preparation method and application thereof |
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