CN106421414B - Preparation process of dendrobium officinale freeze-dried powder - Google Patents
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/898—Orchidaceae (Orchid family)
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- A61K9/00—Medicinal preparations characterised by special physical form
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- A61K9/19—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The invention discloses a preparation process of dendrobium officinale freeze-dried powder, which comprises the following steps: (1) preparing raw materials: taking the dendrobium officinale which meets the standard, washing with water, removing impurities, and rinsing with purified water; (2) cutting into blocks: mechanically cutting into sections, and cutting into 2-4 cm; (3) crushing and pulping: according to the solid-liquid ratio of 1 g: (80-120) adding pure water in a proportion of ml for crushing and pulping, and filtering by a filter screen of 28-32 meshes to receive the juice; (4) and (3) vacuum drying: taking the juice, pre-freezing overnight at-18 to-20 ℃, then carrying out vacuum freeze drying for 16 to 22 hours, and finally sublimating for 12 to 18 hours; (5) crushing: and (4) crushing the freeze-dried powder obtained in the step (4) in order, and sieving particles with a 70-90-mesh sieve to obtain the freeze-dried powder. Compared with the prior art, the method disclosed by the invention is simple to operate, the steps are scientific and reasonable, and no solvent pollution or residue exists in the preparation process of the dendrobium officinale freeze-dried powder; the preparation temperature is low, and the biological activity of functional substances in the dendrobium officinale is ensured not to be lost.
Description
Technical Field
The invention relates to a preparation process of dendrobium officinale freeze-dried powder, and belongs to the technical field of pharmaceutical preparations.
Background
The dendrobium officinale products sold in the market at present are prepared by firstly preparing stems into dry products, namely dendrobium officinale, which are cut off leaves and fibrous roots of the dendrobium officinale and then are twisted into spiral or spring-shaped dry products while being dried; secondly, directly selling fresh products including stems, flowers and leaves; and thirdly, finely and deeply processed products which mainly comprise medicines and health-care foods in types of granules, capsules, extractum, oral liquid, buccal tablets, tea, compound preparations and the like. Various types of health-care foods are developed, and most of the health-care foods are composite health-care products added with other components. Dendrobium officinale health food generally comprises more than 2 medicinal materials (containing Dendrobium officinale), and health food prepared from single dendrobium officinale is rare. Firstly, considering that the price of the dendrobium officinale is high, the daily dose for achieving the same effect is large when the dendrobium officinale is singly used, and the product price is high, so that the dendrobium officinale can not be born by common consumers. Secondly, based on the basic theory of traditional Chinese medicine, the maximum curative effect is exerted through the compatibility of the traditional Chinese medicines, so that the health care effect is more prominent.
Traditionally, dendrobium officinale is usually used as a medicinal material in the form of dry dendrobium candidum, and is mainly taken in the form of water boiling and decoction. The main active ingredient polysaccharide content and efficacy may be affected by a number of factors in the process.
Different drying methods obviously affect the content of dendrobium officinale polysaccharide. Plum smart and the like adopt 4 methods of direct drying, drying after scalding, drying while rubbing, and drying while rubbing after scalding, and polysaccharide content is measured after drying at different temperatures (100 ℃, 80 ℃, 60 ℃, and room temperature), and the results show that the mass fraction of the polysaccharide of the dendrobium officinale medicinal material obtained by different post-harvest processing methods is 26.59-32.70%, and the polysaccharide content of the dendrobium officinale medicinal material treated by drying at 100 ℃ and 80 ℃ while rubbing is the highest, respectively 32.70% and 32.58%; the polysaccharide content of the medicinal material after direct drying at 60 ℃ is the lowest, and is 26.59%. Modern pharmacology and clinical prove that timely harvesting, reasonable drying and scientific processing of traditional Chinese medicinal materials are important ways for ensuring and improving the quality of the medicinal materials. Researches such as Xinming and the like show that the polysaccharide content after the dendrobium officinale is dried is arranged in a hot air drying mode, namely vacuum drying, vacuum freeze drying and natural drying mode, wherein the polysaccharide content of the dendrobium officinale subjected to hot air drying is the highest and reaches 31.13%; the polysaccharide content under natural drying conditions is the lowest, 20.72%. But the studies of the standing drill and the like consider that compared with the traditional processing mode, the mechanical processing has little influence on the polysaccharide content.
The related products of the dendrobium officinale and the preparation process thereof also have a plurality of invention patents, the dosage forms of the products are various, and the related preparations of the dendrobium officinale and the related patent dosage forms of the application relate to traditional dosage forms such as capsules, tablets, granules, oral liquid, powder, buccal tablets and the like through the database search of the patent office.
At present, the development of a lot of dendrobium officinale products is only in a low level of primary processing, but deep processing products are insufficient or new products are not developed sufficiently, and additionally, because the dendrobium officinale has higher commercial value, the propaganda of the dendrobium officinale products on the market is exaggerated too much, so that the phenomenon of being filled with dendrobium officinale is endless.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the technical problems, the invention provides a preparation process of dendrobium officinale freeze-dried powder and a method for preparing buccal tablets by using the dendrobium officinale freeze-dried powder.
The technical scheme is as follows: in order to realize the aim, the invention discloses a preparation process of dendrobium officinale freeze-dried powder, which comprises the following steps:
(1) preparing raw materials: taking the dendrobium officinale which meets the standard, washing with water, removing impurities, and rinsing with purified water;
(2) cutting into blocks: mechanically cutting into sections, and cutting into 2-4 cm;
(3) crushing and pulping: according to the solid-liquid ratio of 1 g: (80-120) adding pure water in a proportion of ml for crushing and pulping, and filtering by a filter screen of 28-32 meshes to receive the juice;
(4) and (3) vacuum drying: taking the juice, pre-freezing overnight at-18 to-20 ℃, then carrying out vacuum freeze drying for 16 to 22 hours, and finally sublimating for 12 to 18 hours;
(5) crushing: and (4) crushing the freeze-dried powder obtained in the step (4) in order, and sieving particles with a 70-90-mesh sieve to obtain the freeze-dried powder.
Preferably, the compliance criteria in step (1) is compliance with the requirements of pharmacopoeia of the people's republic of china (2015 edition).
As another preference, the conditions for the pulverization in the step (3) are: crushing rotating speed: 2500-: 38-42 ℃.
As another preferred mode, in the step (4), the temperature of the cold trap is set to be-24 to-28 ℃ and the vacuum degree is set to be-1.1 to-0.1 Pa during the vacuum freeze drying.
Preferably, the sublimation temperature in the step (4) is 38-48 ℃.
The invention also provides a preparation process of the dendrobium officinale freeze-dried powder buccal tablets, which comprises the following steps:
(1) preparing the dendrobium officinale freeze-dried powder according to the preparation process;
(2) mixing the lyophilized powder with adjuvants to obtain mixture;
(3) and (3) adding a lubricant into the mixture, fully and uniformly mixing, and tabletting to obtain the tablet.
Preferably, the auxiliary materials in the step (2) are isomalt, corn starch and lactose.
As another preference, the lubricant in step (3) is magnesium stearate.
Further preferably, the weight parts of the raw materials are as follows:
5-286.4 parts of dendrobium officinale freeze-dried powder, 1.0-60 parts of isomaltitol, 0.5-28 parts of corn starch,
0.8-20 parts of lactose and 0.1-5.6 parts of magnesium stearate.
The preparation process of the invention selects the optimal water content and particle size of low-temperature pulping, freeze-drying time, airflow crushing flow and the like. Compared with similar products produced by other methods, the obtained dendrobium officinale freeze-dried powder is more enriched in dendrobium officinale active ingredients, and can also keep the original taste and color of dendrobium officinale.
The dendrobium officinale freeze-dried powder buccal tablet prepared by the preparation process only takes a dendrobium officinale freeze-dried powder as a main raw material, highlights the health care effect of dendrobium officinale and simultaneously does not lose the original taste and color. The dendrobium officinale freeze-dried powder buccal tablet with the immunity-enhancing and health-care effects is prepared by using the dendrobium officinale freeze-dried powder and adding a proper amount of auxiliary materials such as isomaltitol, edible corn starch, lactose, magnesium stearate and the like into the dendrobium officinale freeze-dried powder, and is prepared by main processes such as blending, mixing, tabletting, packaging and the like, and the dendrobium officinale freeze-dried powder buccal tablet has the polysaccharide content of more than 18g/100g and strong stability.
Has the advantages that: compared with the prior art, the method disclosed by the invention is simple to operate, the steps are scientific and reasonable, and no solvent pollution or residue exists in the preparation process of the dendrobium officinale freeze-dried powder; the preparation temperature is low, and the biological activity of functional substances in the dendrobium officinale is ensured not to be lost. Compared with similar products, the dendrobium officinale dry powder buccal tablet has high content of dendrobium polysaccharide and can better keep the biological activity of the dendrobium polysaccharide.
Detailed Description
Example 1
The preparation process of the dendrobium officinale freeze-dried powder comprises the following steps:
(1) preparing raw materials: taking the dendrobium officinale which meets the requirements of pharmacopoeia of the people's republic of China (2015 edition), washing with water, removing impurities, and rinsing with purified water;
(2) cutting into blocks: mechanically cutting into sections, and cutting into 2-4 cm;
(3) crushing and pulping: according to the solid-liquid ratio of 1 g: adding pure water into 100ml of the mixture for crushing and pulping, wherein the crushing rotating speed is as follows: 3000rpm, operating temperature: filtering with 30 mesh sieve at 40 deg.C to obtain juice;
(4) and (3) vacuum drying: taking the juice, pre-freezing overnight at-18 to-20 ℃, then carrying out vacuum freeze drying, setting the temperature of a cold trap at-26 ℃, the vacuum degree at-0.9 to-0.1 Pa, carrying out freeze drying for 18h, and finally sublimating for 14h, wherein the sublimation temperature is 40 to 45 ℃;
(5) crushing: and (4) crushing the freeze-dried powder obtained in the step (4) in order, and sieving particles with a 80-mesh sieve to obtain the freeze-dried powder.
Example 2
The preparation process of the dendrobium officinale freeze-dried powder is the same as that in example 1, and is different from the following steps: the cool drying time in the step (4) is 20h, and the sublimation time is 16 h.
Example 3
The preparation process of the dendrobium officinale freeze-dried powder comprises the following steps:
(1) preparing raw materials: taking the dendrobium officinale which meets the requirements of pharmacopoeia of the people's republic of China (2015 edition), washing with water, removing impurities, and rinsing with purified water;
(2) cutting into blocks: mechanically cutting into sections, and cutting into 2-4 cm;
(3) crushing and pulping: according to the solid-liquid ratio of 1 g: adding pure water into 80ml of the mixture for crushing and pulping, wherein the crushing rotating speed is as follows: 3500rpm, operating temperature: filtering at 42 deg.C with 28 mesh sieve to receive juice;
(4) and (3) vacuum drying: pre-freezing the juice at-18 to-20 ℃ overnight, and then carrying out vacuum freeze drying at the temperature of-24 ℃ in a cold trap, the vacuum degree of-1.1 Pa, the freeze drying time of 16h, and finally sublimating for 12h, wherein the sublimation temperature is 38 ℃;
(5) crushing: and (4) crushing the freeze-dried powder obtained in the step (4) in order, and sieving particles with a 70-mesh sieve to obtain the freeze-dried powder.
Example 4
The preparation process of the dendrobium officinale freeze-dried powder comprises the following steps:
(1) preparing raw materials: taking the dendrobium officinale which meets the requirements of pharmacopoeia of the people's republic of China (2015 edition), washing with water, removing impurities, and rinsing with purified water;
(2) cutting into blocks: mechanically cutting into sections, and cutting into 2-4 cm;
(3) crushing and pulping: according to the solid-liquid ratio of 1 g: adding pure water into 120ml of the mixture for crushing and pulping, wherein the crushing rotating speed is as follows: 2500rpm, operating temperature: filtering with 32 mesh sieve at 38 deg.C to obtain juice;
(4) and (3) vacuum drying: pre-freezing the juice at-18 to-20 ℃ overnight, and then carrying out vacuum freeze drying at the temperature of-28 ℃ of a cold trap, the vacuum degree of-0.1 Pa, the freeze drying time of 22h, and finally sublimating for 18h, wherein the sublimation temperature is 48 ℃; (5) crushing: and (4) crushing the freeze-dried powder obtained in the step (4) in order, and sieving particles with a 90-mesh sieve to obtain the freeze-dried powder.
Example 5
Preparing the dendrobium officinale freeze-dried powder buccal tablets: the dendrobium officinale freeze-dried powder is obtained by the method of the embodiment 1.
Prescription:
5 parts of dendrobium officinale freeze-dried powder, 60 parts of isomaltitol, 28 parts of corn starch,
20 parts of lactose and 5.6 parts of magnesium stearate.
The preparation process comprises the following steps:
(1) taking the dendrobium officinale freeze-dried powder, and fully mixing the dendrobium officinale freeze-dried powder with isomaltitol, corn starch and lactose to obtain a mixture;
(2) and adding magnesium stearate into the mixture, fully and uniformly mixing, and tabletting to obtain the tablet.
Example 6
Preparing the dendrobium officinale freeze-dried powder buccal tablets: the dendrobium officinale freeze-dried powder is obtained by the method of the embodiment 1.
Prescription:
286.4 parts of dendrobium officinale freeze-dried powder, 60 parts of isomaltitol, 28 parts of corn starch,
20 parts of lactose and 5.6 parts of magnesium stearate.
The preparation process comprises the following steps:
(1) taking the dendrobium officinale freeze-dried powder, and fully mixing the dendrobium officinale freeze-dried powder with isomaltitol, corn starch and lactose to obtain a mixture;
(2) and adding magnesium stearate into the mixture, fully and uniformly mixing, and tabletting to obtain the tablet.
Example 7
Preparing the dendrobium officinale freeze-dried powder buccal tablets: the dendrobium officinale freeze-dried powder is obtained by the method in the embodiment 2.
Prescription:
286.4 parts of dendrobium officinale freeze-dried powder, 1.0 part of isomaltitol, 0.5 part of corn starch,
0.8 part of lactose and 0.1 part of magnesium stearate.
The preparation process comprises the following steps:
(1) taking the dendrobium officinale freeze-dried powder, and fully mixing the dendrobium officinale freeze-dried powder with isomaltitol, corn starch and lactose to obtain a mixture;
(2) and adding magnesium stearate into the mixture, fully and uniformly mixing, and tabletting to obtain the tablet.
Example 8
Preparing the dendrobium officinale freeze-dried powder buccal tablets: the dendrobium officinale freeze-dried powder is obtained by the method of the embodiment 1.
Prescription:
145.7 parts of dendrobium officinale freeze-dried powder, 35 parts of isomaltitol, 14 parts of corn starch,
10 parts of lactose and 2.8 parts of magnesium stearate.
The preparation process comprises the following steps:
(1) taking the dendrobium officinale freeze-dried powder, and fully mixing the dendrobium officinale freeze-dried powder with isomaltitol, corn starch and lactose to obtain a mixture;
(2) and adding magnesium stearate into the mixture, fully and uniformly mixing, and tabletting to obtain the tablet.
Experimental example 1 determination of polysaccharide content in dendrobium officinale freeze-dried powder
The polysaccharide quality before the dendrobium officinale treatment and after the dendrobium officinale is prepared into freeze-dried powder is measured by adopting a concentrated sulfuric acid method, and the measurement results are shown in the following table 1.
The control 1 group was identical to the inventive example 1 except that: the solid-liquid ratio during crushing and pulping is 1 g: 5ml, conditions for vacuum freeze drying were: vacuum freeze-drying at-56 deg.C under vacuum degree of 7-9Pa for 20 hr, and keeping the same for the rest;
the control 2 group was identical to the inventive example 1 except that: the solid-liquid ratio during crushing and pulping is 1 g: 5ml, the rest are the same;
the same batches of dendrobium officinale raw materials (500g) with the same weight are taken for processing in each group, and the measurement results are as follows 1:
TABLE 1 measurement of polysaccharide content
The results in the table 1 show that compared with the two control groups, the polysaccharide quality of the freeze-dried powder prepared by the preparation process is only reduced by about 1%, and almost no loss exists; the quality of the polysaccharide in the two control groups is reduced by more than 16 percent, and the loss degree of the polysaccharide is high.
Experimental example 2 study on stability of dendrobium officinale freeze-dried powder buccal tablets
And (3) determining the polysaccharide content in the dendrobium officinale freeze-dried powder buccal tablets by adopting a concentrated sulfuric acid method.
The control group is the same as the control group in the experimental example 1, and the obtained freeze-dried powder is used for preparing the freeze-dried powder buccal tablets.
The stability of the dendrobium officinale freeze-dried powder buccal tablet is investigated by adopting an accelerated test, and the results are shown in the following table 2:
TABLE 2 stability study of lyophilized powder of Dendrobium officinale Kimura et Migo buccal tablets
Compared with two control groups, the freeze-dried powder buccal tablet prepared by the preparation process has the advantages that the polysaccharide content is not obviously changed in 1 month, 3 months and 6 months, and the stability and the performance are high. The polysaccharide content of the two control products is as high as 5.2g/100g, which is the most polysaccharide loss.
Claims (7)
1. A preparation process of dendrobium officinale freeze-dried powder is characterized by comprising the following steps:
(1) preparing raw materials: taking the dendrobium officinale which meets the standard, washing with water, removing impurities, and rinsing with purified water;
(2) cutting into blocks: mechanically cutting into sections, and cutting into 2-4 cm;
(3) crushing and pulping: according to the solid-liquid ratio of 1 g: (80-120) ml of pure water is added for crushing and pulping, and the operation temperature is as follows: filtering at 38-42 deg.C with 28-32 mesh sieve to obtain juice;
(4) and (3) vacuum drying: taking the juice, pre-freezing overnight at-18 to-20 ℃, then carrying out vacuum freeze drying, setting the temperature of a cold trap at-24 to-28 ℃, the vacuum degree at-1.1 to-0.1 Pa, carrying out freeze drying for 16 to 22 hours, and finally sublimating for 12 to 18 hours;
(5) crushing: and (4) crushing the freeze-dried powder obtained in the step (4) in order, and sieving particles with a 70-90-mesh sieve to obtain the freeze-dried powder.
2. The preparation process of the dendrobium officinale freeze-dried powder according to claim 1, wherein the compliance standard in the step (1) is in accordance with the requirements of pharmacopoeia of the people's republic of China (2015 edition).
3. The preparation process of the dendrobium officinale freeze-dried powder according to claim 1, wherein the crushing conditions in the step (3) are as follows: crushing rotating speed: 2500-: 38-42 ℃.
4. The preparation process of the dendrobium officinale freeze-dried powder according to claim 1, wherein the sublimation temperature in the step (4) is 38-48 ℃.
5. A preparation process of dendrobium officinale freeze-dried powder buccal tablets is characterized by comprising the following steps:
(1) preparing the dendrobium officinale freeze-dried powder according to the preparation process of any one of claims 1-4;
(2) mixing the lyophilized powder with adjuvants to obtain mixture;
(3) and (3) adding a lubricant into the mixture, fully and uniformly mixing, and tabletting to obtain the tablet.
6. The preparation process of the dendrobium officinale freeze-dried powder buccal tablet according to claim 5, wherein the auxiliary materials in the step (2) are isomalt, corn starch and lactose.
7. The preparation process of the dendrobium officinale freeze-dried powder buccal tablet according to claim 5, wherein the lubricant in the step (3) is magnesium stearate.
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| CN106692703A (en) * | 2017-03-17 | 2017-05-24 | 贵州健瑞安药业有限公司 | Preparation method of dendrobium freeze-dried powder |
| CN106822605A (en) * | 2017-03-31 | 2017-06-13 | 泸州德高生物科技有限公司 | The preparation method of the ecological oral freeze-dried powder of the stem of noble dendrobium |
| CN107802744A (en) * | 2017-11-01 | 2018-03-16 | 浙江龙之源生物科技有限公司 | A kind of dendrobium candidum freeze-dried powder manufacture craft |
| CN108030131B (en) * | 2017-12-20 | 2020-08-25 | 普洱云福生物科技有限公司 | Processing method of dendrobium officinale refined slices |
| CN108902975A (en) * | 2018-07-24 | 2018-11-30 | 浙江兰溪锦荣生物科技股份有限公司 | A kind of production technology of dendrobium candidum dried frozen aquatic products |
| CN108926677A (en) * | 2018-08-20 | 2018-12-04 | 云南和瑾科技有限公司 | A kind of dendrobium nobile freeze-drying powder producing method |
| CN109260122A (en) * | 2018-11-28 | 2019-01-25 | 衡水学院 | A kind of whitening anti-aging cosmetics and preparation method thereof |
| CN114963745A (en) * | 2022-05-23 | 2022-08-30 | 舟山市食品药品检验检测研究院 | Optimized processing technology for dendrobium officinale produced in Zhejiang |
| CN115251377A (en) * | 2022-08-08 | 2022-11-01 | 江西省农业科学院农产品加工研究所 | Dendrobium officinale instant food and preparation method thereof |
| CN115251378A (en) * | 2022-08-08 | 2022-11-01 | 江西省农业科学院农产品加工研究所 | Dendrobium officinale microcapsule and preparation method thereof |
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| CN104223063A (en) * | 2014-08-26 | 2014-12-24 | 北京林业大学 | Freeze-dried dendrobium officinale powder and preparation method thereof |
| CN104758257B (en) * | 2015-04-02 | 2017-08-22 | 贵州同威生物科技有限公司 | Fresh dendrobium candidum freeze-dried powder and preparation method |
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