CN106674370A - Bletilla striata gelatin and preparation method thereof - Google Patents

Bletilla striata gelatin and preparation method thereof Download PDF

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Publication number
CN106674370A
CN106674370A CN201710060316.3A CN201710060316A CN106674370A CN 106674370 A CN106674370 A CN 106674370A CN 201710060316 A CN201710060316 A CN 201710060316A CN 106674370 A CN106674370 A CN 106674370A
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Prior art keywords
bletillae
filtrate
bletilla glucomannan
rhizoma bletillae
pseudobulbus bletillae
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晏前海
龙娴郦
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Guizhou Province Wuling Yam Plant Bletilla Development Co Ltd
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Guizhou Province Wuling Yam Plant Bletilla Development Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Molecular Biology (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Sustainable Development (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention relates to a bletilla striata gelatin and a preparation method thereof, which relate to the technical field of biopharmaceutics. The preparation method of the bletilla striata gelatin comprises the steps of a smashing step, a screening step, an extracting step and a purifying step. The preparation method of the bletilla striata gelatin comprises the concrete steps of smashing bletilla striata, then screening through a saturated sodium chloride solution, adding water for ultrasonic processing after screening, and purifying through an ethanol solution. According to the method, the bletilla striata raw materials are well screened, and the prepared bletilla striata gelatin has high purity and a good pharmacological function; the extraction rate of the bletilla striata gelatin is greatly improved, the utilization ratio of the raw materials is improved, and the cost is reduced. The bletilla striata gelatin provided by the invention is prepared through the preparation method of the bletilla striata gelatin, and has high purity and a good pharmacological function.

Description

Bletilla glucomannan and preparation method thereof
Technical field
The present invention relates to biopharmacy technical field, more particularly to a kind of Bletilla glucomannan and preparation method thereof.
Background technology
The Pseudobulbus Bletillae (Rhizoma Bletillae) is used as convergence, hemorrhage application is long-standing, and haemostatic effect is definitely reliable, and its mechanism of action is demonstrate,proved with it The substantial amounts of Bletilla glucomannan that the bright dissolving with shortening clotting time, suppression human body to cellulose is made to contain is relevant.Pseudobulbus Bletillae (Rhizoma Bletillae) quality stick it is greasy, Containing colloid, it can improve local blood circulation, promote epithelial cell reparation, can stop blooding, sore, skin moistening and granulation promoting.The Pseudobulbus Bletillae (Rhizoma Bletillae) carries Take thing also to be used by experiment, artificial thrombosis can be quickly formed, not only trauma hemostasis are commonly used, and also have preferable effect to visceral hemorrhage. The Pseudobulbus Bletillae (Rhizoma Bletillae) has and significantly promote keratinocyte effect, and this rush migration effect is to treating skin trauma, hemostasis and immediate union Have a major impact, further illustrate reparation and metabolic process that Bletilla glucomannan directly take part in damaged tissues or cell.
Decoction and alcohol sedimentation technique is mainly currently for the extracting method of Bletilla glucomannan.Inventors herein have recognized that:Current water Carry alcohol deposition method and there is no screening function to Pseudobulbus Bletillae (Rhizoma Bletillae) raw material, in obtained Bletilla glucomannan finished product harmful substance is easily mixed into, have a strong impact on The quality and pharmacological effect of Bletilla glucomannan.On the other hand, the Bletilla glucomannan extraction ratio of Pseudobulbus Bletillae (Rhizoma Bletillae) raw material is not in current decoction and alcohol sedimentation technique Height, raw material availability is low, causes cost to increase.
The content of the invention
It is an object of the invention to provide a kind of preparation method of Bletilla glucomannan, this method has to Pseudobulbus Bletillae (Rhizoma Bletillae) raw material preferably screen work( Can, obtained Bletilla glucomannan purity is high, good drug efficacy;And the extraction ratio of Bletilla glucomannan can be greatly improved, raw material availability is improved, is reduced Cost.
Another object of the present invention is to provide a kind of Bletilla glucomannan, the Bletilla glucomannan purity is high, and pharmacological effect is good.
The present invention solves its technical problem and employs the following technical solutions to realize.
The present invention proposes a kind of preparation method of Bletilla glucomannan, including:
Pulverising step:The clean Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity for 10-100 mesh;
Screening step:During the Pseudobulbus Bletillae (Rhizoma Bletillae) after crushing is added into weight for 4-6 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight of saturated nacl aqueous solution, mix Even standing 5-10 minutes;
The floating thing for floating on liquid level is skimmed, the first filtering residue and the first filtrate is filtered to obtain;
Extraction step:Added water at least one times supersound process to the first filtering residue, and the supersound process that adds water every time is by with lower section Formula is carried out:Addition weight is the water of 8-12 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight in the first filtering residue, and ultrasonic 1-2 hours filter to get filtrate, and merge The filtrate obtained by supersound process that adds water every time obtains the second filtrate;
Purification step:Ethanol being added to the second filtrate and mixing to obtain alcohol deposit fluid, the mass concentration of ethanol is in alcohol deposit fluid 50%-80%;
By alcohol deposit fluid standing sedimentation 8-12 hours, precipitum is collected by filtration and is dried, obtain Bletilla glucomannan.
The present invention proposes a kind of Bletilla glucomannan, is obtained according to the preparation method of above-mentioned Rhizoma Bletillae gel.
The preparation method of the Rhizoma Bletillae gel of the embodiment of the present invention and the beneficial effect of Rhizoma Bletillae gel are:The preparation side of the Rhizoma Bletillae gel In pulverising step by Pseudobulbus Bletillae (Rhizoma Bletillae) raw material pulverizing, improve Bletilla glucomannan oozes out effect and extraction effect to method;And Pseudobulbus Bletillae (Rhizoma Bletillae) raw material is abundant After crushing, the part that may be present inferior inside Pseudobulbus Bletillae (Rhizoma Bletillae) raw material and/or lesion portion is fully exposed, be conducive in screening step Rapid middle specificity simultaneously fully screens out poor quality part and/or lesion portion, improves the quality of Pseudobulbus Bletillae (Rhizoma Bletillae) raw material, makes the obtained Pseudobulbus Bletillae (Rhizoma Bletillae) Glue has higher purity and pharmacological effect, while the screening step is avoided screens out the raw material for causing to Pseudobulbus Bletillae (Rhizoma Bletillae) stem block entirety Waste.In screening step, the sodium chloride solution of saturation has antibacterial, bactericidal action to Pseudobulbus Bletillae (Rhizoma Bletillae) material, while the Pseudobulbus Bletillae (Rhizoma Bletillae) can be made Raw material is dehydrated, and after adding water again in extraction step, the cell wall that Pseudobulbus Bletillae (Rhizoma Bletillae) Jing dehydrations cause the Pseudobulbus Bletillae (Rhizoma Bletillae) with water absorption course is more It is broken, be conducive to improving the extraction ratio of Bletilla glucomannan;Carry out ultrasound procedure plus to the Pseudobulbus Bletillae (Rhizoma Bletillae) so that the cell wall of the Pseudobulbus Bletillae (Rhizoma Bletillae) it is broken Rate is higher, further increases the extraction ratio of Bletilla glucomannan.This method has preferable screening function, obtained Bletilla glucomannan to Pseudobulbus Bletillae (Rhizoma Bletillae) raw material Purity is high, good drug efficacy;And the extraction ratio of Bletilla glucomannan can be greatly improved, the utilization rate of raw material is improved, production cost is reduced.
The Bletilla glucomannan that the present invention is provided is obtained by above-mentioned preparation method, and the Bletilla glucomannan purity is high, and pharmacological effect is good.
Specific embodiment
To make purpose, technical scheme and the advantage of the embodiment of the present invention clearer, below will be in the embodiment of the present invention Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, being can pass through the conventional product that commercially available purchase is obtained Product.
The preparation method and Bletilla glucomannan of the Bletilla glucomannan of the embodiment of the present invention are specifically described below.
A kind of preparation method of Bletilla glucomannan, including:
Pulverising step:The clean Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity for 10-100 mesh.
Screening step:During the Pseudobulbus Bletillae (Rhizoma Bletillae) after crushing is added into weight for 4-6 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight of saturated nacl aqueous solution, mix Even standing 5-10 minutes.
The floating thing for floating on liquid level is skimmed, the first filtering residue and the first filtrate is filtered to obtain.
Extraction step:Added water at least one times supersound process to the first filtering residue, and the supersound process that adds water every time is by with lower section Formula is carried out:Addition weight is the water of 8-12 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight in the first filtering residue, and ultrasonic 1-2 hours filter to get filtrate, and merge The filtrate obtained by supersound process that adds water every time obtains the second filtrate.
Purification step:Ethanol being added to the second filtrate and mixing to obtain alcohol deposit fluid, the mass concentration of ethanol is in alcohol deposit fluid 50%-80%.
By alcohol deposit fluid standing sedimentation 8-12 hours, precipitum is collected by filtration and is dried, obtain Bletilla glucomannan.
Wherein:
In pulverising step, it is 10-100 mesh that the Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity, on the one hand ensures that the Pseudobulbus Bletillae (Rhizoma Bletillae) can obtain sufficient powder It is broken, to improve the extraction ratio of Bletilla glucomannan;On the other hand also cause the Pseudobulbus Bletillae (Rhizoma Bletillae) after crushed still can be by normal filtration, in order to avoid in grain Spend hour and occur in situation about cannot be filtered out through filter opening in filter process.Additionally, the Pseudobulbus Bletillae (Rhizoma Bletillae) is through crushing, can be with Make the medical material inside the Pseudobulbus Bletillae (Rhizoma Bletillae) fully come out, can particularly make Pseudobulbus Bletillae (Rhizoma Bletillae) inside lesion portion that may be present and/or poor quality Part is fully come out, and is easy to fully screen out lesion portion and/or part inferior in follow-up screening step, while can Avoid screening out the waste of material that whole Pseudobulbus Bletillae (Rhizoma Bletillae) stem block is caused.
It is 4-6 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight of saturated nacl aqueous solution by the Pseudobulbus Bletillae (Rhizoma Bletillae) addition weight after crushing in screening step, mixes Even standing 5-10 minutes.After standing, because part inferior and/or lesion portion infect its composition and are sucked by acarid class pest, Micro-bubble is internally formed, global density is relatively low, liquid level will be floated in saturated nacl aqueous solution;Not with lesion Point and/or part inferior the Pseudobulbus Bletillae (Rhizoma Bletillae) due to density it is larger, be sunken to bottom.By skimming the floating thing and/or drift that float on liquid level Float, you can screen out lesion portion and/or part inferior.By the step, can not only realize to lesion portion and/or poor quality It is partial fully to screen out and be avoided that the waste that screens out whole Pseudobulbus Bletillae (Rhizoma Bletillae) stem block to raw material, and saturated nacl aqueous solution is to Pseudobulbus Bletillae (Rhizoma Bletillae) material With antibacterial, bactericidal action, it is ensured that the Pseudobulbus Bletillae (Rhizoma Bletillae) and Bletilla glucomannan pharmacologically active, and other impurity will not be introduced.One Aspect improves the purity and pharmacological effect of the Pseudobulbus Bletillae (Rhizoma Bletillae) and Bletilla glucomannan, on the other hand improves the safety of the Pseudobulbus Bletillae (Rhizoma Bletillae) and Bletilla glucomannan Property.
The remainder for having skimmed lesion portion and/or part inferior is filtered, the first filtering residue and the first filtrate is obtained.
In extraction step, added water at least one times supersound process to the first filtering residue.Because the first filtering residue is Jing screening steps Rapid to be obtained, in screening step, the Pseudobulbus Bletillae (Rhizoma Bletillae) occurs to be dehydrated and be in shrivelled shape in saturated nacl aqueous solution, as the first filtering residue.To After first filtering residue adds water, due to osmosiss, the first filtering residue absorbs water and in saturation shape.Jing dehydration and again after water absorption course, the The cell wall of the Pseudobulbus Bletillae (Rhizoma Bletillae) of one filtering residue is easy to rupture, and this is conducive to oozing out for Bletilla glucomannan, improves the extraction ratio of Bletilla glucomannan.
On the other hand, because the first filtering residue is Jing after dehydration and again water absorption course, its cell wall is easy to rupture, and does not send out The cell wall of raw rupture also becomes quite fragile.First filtering residue, due to the crushing effect of ultrasound, promotes Jing after ultrasound procedure process The cell wall rupture of the Pseudobulbus Bletillae (Rhizoma Bletillae) so that the rupture rate of the cell wall of the Pseudobulbus Bletillae (Rhizoma Bletillae) greatly improves so that Bletilla glucomannan oozes out effect more preferably, Further increase the extraction ratio of Bletilla glucomannan.
Additionally, supersound process is conducive to accelerating oozing out for Bletilla glucomannan, Bletilla glucomannan is quickly oozed out from Pseudobulbus Bletillae (Rhizoma Bletillae) cell, improve The yield oozed out speed and leaching rate, improve Bletilla glucomannan of Bletilla glucomannan.
The filtrate obtained after the supersound process that adds water every time is merged and obtains the second filtrate, the Bletilla glucomannan content in the second filtrate It is just very high.
In purification step, add ethanol to the second filtrate and mix to obtain alcohol deposit fluid, and after standing sedimentation 8-12 hours, a side Face, because Bletilla glucomannan does not dissolve in ethanol, Bletilla glucomannan can fall to the bottom of alcohol deposit fluid, and other organic substances in the second filtrate The material for being dissolved in organic faciess with other will be dissolved in the middle of ethanol, realized to Bletilla glucomannan and other Organic substances and/or Bletilla glucomannan The material for being dissolved in organic faciess with other is separated;On the other hand, ethanol is used as the further antibacterial, sterilization of the Bletilla glucomannan to extracting, Substantially increase the purity of Bletilla glucomannan, it is ensured that the normal pharmacologic effect of Bletilla glucomannan.
During made above, whole process will not be damaged to the Pseudobulbus Bletillae (Rhizoma Bletillae) and/or Bletilla glucomannan, and the preparation method exists Largely ensure that the pharmacologically active of the Pseudobulbus Bletillae (Rhizoma Bletillae) and Bletilla glucomannan.This method has preferable screening function to Pseudobulbus Bletillae (Rhizoma Bletillae) raw material, is obtained Bletilla glucomannan purity is high, good drug efficacy;And the extraction ratio of Bletilla glucomannan can be greatly improved, the utilization rate of raw material is improved, production is reduced Cost.
Further, also included before purification step, the first filtrate is removed in Sodium Chloride and water using dialysis, receive The step of collecting residue and residue be dissolved in into the second filtrate.
The component in the first filtrate can be realized separating using dialysis, that is, be separated into two parts, first part It is sodium chloride solution for water and Sodium Chloride;The second part is Bletilla glucomannan.The Pseudobulbus Bletillae (Rhizoma Bletillae) that will be obtained from the first filtrate by dialysis Glue is added in the second filtrate, can improve extraction ratio and utilization rate to the Bletilla glucomannan in the Pseudobulbus Bletillae (Rhizoma Bletillae), is reduced in screening process The loss of bad student.The extraction ratio of Bletilla glucomannan is improve from another point of view, has saved cost.
Further, also included before pulverising step:The Pseudobulbus Bletillae (Rhizoma Bletillae) is wrapped up with plant ash, after stirring 10-30 minutes clear water is used The cleaning Pseudobulbus Bletillae (Rhizoma Bletillae).
The Pseudobulbus Bletillae (Rhizoma Bletillae) is easily encroached in growth course by insects such as acarids, particularly has to the tuber of the Pseudobulbus Bletillae (Rhizoma Bletillae) tighter The corrosion harmfulness of weight.The Pseudobulbus Bletillae (Rhizoma Bletillae) is wrapped up with plant ash, and is stirred or is rubbed 10-30 minutes, effectively the Pseudobulbus Bletillae (Rhizoma Bletillae) can be suffered into demodicid mite The part of worm corrosion is cleaned out, and plant ash has sterilization antiseptical function, and Jing after clear water is cleaned, the incident acarid of the Pseudobulbus Bletillae (Rhizoma Bletillae) is rotten The part of erosion can be cleaned.Improve purity and the safety of Pseudobulbus Bletillae (Rhizoma Bletillae) raw material, so improve the purity of Bletilla glucomannan with Safety, it is ensured that the normal pharmacologic effect of Bletilla glucomannan.
Further, peeling step was also included before pulverising step, peeling step is carried out in the following manner:
Under the conditions of 30 DEG C -50 DEG C, the Pseudobulbus Bletillae (Rhizoma Bletillae) is soaked in into the ethanol solution 10min- of the hydrochloric acid that mass concentration is 3%-8% 20min, stirring.
The floating thing for floating on liquid level is skimmed, the Pseudobulbus Bletillae (Rhizoma Bletillae) is pulled out and is used clean water.
This peeling step is soaked using the ethanol solution of hydrochloric acid to Pseudobulbus Bletillae (Rhizoma Bletillae) so that the skin Automatic-falling of the Pseudobulbus Bletillae (Rhizoma Bletillae), is coordinated To stir, depart from can Pseudobulbus Bletillae (Rhizoma Bletillae) skin more thorough.During this peeling, can't be to the Pseudobulbus Bletillae (Rhizoma Bletillae) and the normal pharmacologic of Bletilla glucomannan Matter is produced to be affected or destroys, and acid bad border is conducive to the preservation of Bletilla glucomannan and stablizes.On the one hand by the removing of Pseudobulbus Bletillae (Rhizoma Bletillae) skin deep layer, The extraction ratio of Bletilla glucomannan is improve, on the other hand makes Bletilla glucomannan more stable and not easy in inactivation, make the normal pharmacologic effect of Bletilla glucomannan It is guaranteed.
Further, also it is included in before the supersound process that adds water, by 1-2 times that the first filtering residue weight is Pseudobulbus Bletillae (Rhizoma Bletillae) weight The step of water immersion 4-6 hours.
Before the extraction step water dip operation is carried out to the Pseudobulbus Bletillae (Rhizoma Bletillae), be conducive to making the Pseudobulbus Bletillae (Rhizoma Bletillae) fully absorb water.Because the Pseudobulbus Bletillae (Rhizoma Bletillae) is in sieve , in shrivelled shape substantially, the 4-6 hours that are soaked in water can make the Pseudobulbus Bletillae (Rhizoma Bletillae) absorb water again and in full shape to select dehydration in step.Pseudobulbus Bletillae (Rhizoma Bletillae) Jing Dehydration and the continuous process for absorbing water so that the cell wall of the Pseudobulbus Bletillae (Rhizoma Bletillae) easily ruptures.After water immersion 4-6 hours, cell wall is broken Bletilla glucomannan in the Pseudobulbus Bletillae (Rhizoma Bletillae) cell for splitting can fully ooze out, and the cell wall of the also uncracked Pseudobulbus Bletillae (Rhizoma Bletillae) cell of cell wall then becomes swollen Swollen fragility.The Pseudobulbus Bletillae (Rhizoma Bletillae) is Jing after water immersion 4-6 hours, then extracted step process, and the cell wall of Pseudobulbus Bletillae (Rhizoma Bletillae) cell can be made abundant or thorough Bottom ruptures, and is conducive to oozing out for Bletilla glucomannan, can greatly improve the extraction ratio of Bletilla glucomannan.The Bletilla glucomannan of reproduction phase homogenous quantities When, the consumption of Pseudobulbus Bletillae (Rhizoma Bletillae) raw material can be greatly reduced, reduce production cost.
Further, in extraction step, the water temperature during supersound process that adds water ultrasound is controlled to 30 DEG C -50 DEG C.
Under this temperature environment, one side Bletilla glucomannan remains in that chemistry and physical stability, and another aspect is higher to be surpassed Sound temperature is conducive to the softening and rupture of the cell wall of Pseudobulbus Bletillae (Rhizoma Bletillae) cell, improves the rupture rate of the cell wall of Pseudobulbus Bletillae (Rhizoma Bletillae) cell, enters one Step improves the leaching rate and extraction ratio of Bletilla glucomannan.And higher ultrasonic temperature also helps liquid phase warm-up movement, improves the Pseudobulbus Bletillae (Rhizoma Bletillae) Glue oozes out speed, it is ensured that Bletilla glucomannan fully oozes out, and improve Bletilla glucomannan ooze out effect.
Further, in extraction step, the number of times of the supersound process that adds water is 1-3 time.
The Pseudobulbus Bletillae (Rhizoma Bletillae) adds water after supersound process Jing 1-3 time, and Bletilla glucomannan oozes out substantially.Particularly through 3 ultrasounds that add water After process, the part that Bletilla glucomannan can be extracted has been oozed out completely substantially, then carries out the supersound process that adds water of more number of times, to carrying The leaching rate of high Bletilla glucomannan has not had positive effect.
Further, the mass concentration of ethanol is 60%-70% in alcohol deposit fluid.
In purification step, when the mass concentration of ethanol is 60%-70% in alcohol deposit fluid, Bletilla glucomannan will be molten insoluble in ethanol Liquid, Bletilla glucomannan will fall to the bottom of alcohol deposit fluid.And other impurity or organic impurities for being dissolved in organic faciess will be dissolved in ethanol Solution, so as to realize Bletilla glucomannan to separate with impurity Bletilla glucomannan is purified.After alcohol deposit fluid is purified, the purity in Bletilla glucomannan is Jing is at a relatively high.Purification step greatly reduces the content that the impurity or organic impurities of organic faciess are dissolved in Bletilla glucomannan, improves The purity of Bletilla glucomannan, it is ensured that the drug effect of Bletilla glucomannan.
Further, also included before purification step:It is 8-12 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight that second filtrate is concentrated into into weight.
It is 8-12 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight partly in order to preventing aqueous in the second filtrate that second filtrate is concentrated into into weight Measuring consumption that is excessive and causing ethanol increases, and so as to reduce the consumption of ethanol, has saved cost.On the other hand, when the second filter When liquid concentration is excessive, Bletilla glucomannan can be separated out with the form such as jelly part, particularly when Bletilla glucomannan is separated out in the form of jelly When, by organic impurities or the impurity of organic faciess can be dissolved in wrap up, so can hinder will using ethanol in purification process Organic impurities are dissolved in the impurity removing of organic faciess, and then the purity of Bletilla glucomannan can be caused relatively low, and can affect Bletilla glucomannan The property of medicine.
The present invention also provides a kind of Bletilla glucomannan, and the Bletilla glucomannan is obtained in the preparation method by above-mentioned Rhizoma Bletillae gel.This is white Splendid achnatherum glue purity is high, and pharmacological effect is good.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of preparation method of Bletilla glucomannan, including:
The Pseudobulbus Bletillae (Rhizoma Bletillae) is wrapped up with plant ash, stirring uses the clean water Pseudobulbus Bletillae (Rhizoma Bletillae) after 10 minutes.
Under the conditions of 30 DEG C, the above-mentioned Pseudobulbus Bletillae (Rhizoma Bletillae) is soaked in into the ethanol solution 10min of the hydrochloric acid that mass concentration is 3%, is stirred; The floating thing for floating on liquid level is skimmed, the Pseudobulbus Bletillae (Rhizoma Bletillae) is pulled out and is used clean water.
The clean Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity for 10 mesh.
During the Pseudobulbus Bletillae (Rhizoma Bletillae) after crushing is added into weight for 6 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight of saturated nacl aqueous solution, mix and stand 5 points Clock;The floating thing for floating on liquid level is skimmed, the first filtering residue and the first filtrate is filtered to obtain.
By the first filtering residue weight is Pseudobulbus Bletillae (Rhizoma Bletillae) weight, 1 times of water soaks 4 hours, to immersion after the first filtering residue carry out 1 The secondary supersound process that adds water, the supersound process that adds water is carried out in the following manner:Weight is added in the first filtrate for the 12 of Pseudobulbus Bletillae (Rhizoma Bletillae) weight Times water, control water temperature and is 30 DEG C of ultrasounds 2 hours, filter to obtain the second filtrate.
First filtrate is removed into Sodium Chloride and water using dialysis, residue is collected and residue is dissolved in into the second filtrate, And it is 8 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight that the second filtrate is concentrated into into weight.
Ethanol being added to the second filtrate after concentration and being mixed, the mass concentration for obtaining ethanol is 50% alcohol deposit fluid;By precipitate with ethanol Liquid standing sedimentation 8 hours, is collected by filtration precipitum and is dried, and obtains Bletilla glucomannan.
Embodiment 2
A kind of preparation method of Bletilla glucomannan, including:
The Pseudobulbus Bletillae (Rhizoma Bletillae) is wrapped up with plant ash, stirring uses the clean water Pseudobulbus Bletillae (Rhizoma Bletillae) after 30 minutes.
Under the conditions of 50 DEG C, the above-mentioned Pseudobulbus Bletillae (Rhizoma Bletillae) is soaked in into the ethanol solution 20min of the hydrochloric acid that mass concentration is 8%, is stirred; The floating thing for floating on liquid level is skimmed, the Pseudobulbus Bletillae (Rhizoma Bletillae) is pulled out and is used clean water.
The clean Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity for 100 mesh.
During the Pseudobulbus Bletillae (Rhizoma Bletillae) after crushing is added into weight for 6 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight of saturated nacl aqueous solution, mix and stand 10 points Clock;The floating thing for floating on liquid level is skimmed, the first filtering residue and the first filtrate is filtered to obtain.
By the first filtering residue weight is Pseudobulbus Bletillae (Rhizoma Bletillae) weight, 1 times of water soaks 6 hours, to immersion after the first filtering residue carry out 3 The secondary supersound process that adds water, the supersound process that adds water is carried out in the following manner:Weight is added in the first filtrate for the 10 of Pseudobulbus Bletillae (Rhizoma Bletillae) weight Times water, control water temperature for 40 DEG C of ultrasounds 1 hour, filter to get filtrate, the merging filtrate obtained by supersound process that adds water every time obtains second Filtrate.
First filtrate is removed into Sodium Chloride and water using dialysis, residue is collected and residue is dissolved in into the second filtrate, And it is 12 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight that the second filtrate is concentrated into into weight.
Ethanol being added to the second filtrate after concentration and being mixed, the mass concentration for obtaining ethanol is 80% alcohol deposit fluid;By alcohol Heavy liquid standing sedimentation 12 hours, is collected by filtration precipitum and is dried, and obtains Bletilla glucomannan.
Embodiment 3
A kind of preparation method of Bletilla glucomannan, including:
The Pseudobulbus Bletillae (Rhizoma Bletillae) is wrapped up with plant ash, stirring uses the clean water Pseudobulbus Bletillae (Rhizoma Bletillae) after 30 minutes.
Under the conditions of 40 DEG C, the above-mentioned Pseudobulbus Bletillae (Rhizoma Bletillae) is soaked in into the ethanol solution 20min of the hydrochloric acid that mass concentration is 8%, is stirred; The floating thing for floating on liquid level is skimmed, the Pseudobulbus Bletillae (Rhizoma Bletillae) is pulled out and is used clean water.
The clean Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity for 100 mesh.
During the Pseudobulbus Bletillae (Rhizoma Bletillae) after crushing is added into weight for 4 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight of saturated nacl aqueous solution, mix and stand 10 points Clock;The floating thing for floating on liquid level is skimmed, the first filtering residue and the first filtrate is filtered to obtain.
By the first filtering residue weight is Pseudobulbus Bletillae (Rhizoma Bletillae) weight, 2 times of water soaks 6 hours, to immersion after the first filtering residue carry out 3 The secondary supersound process that adds water, the supersound process that adds water is carried out in the following manner:Weight is added in the first filtrate for the 12 of Pseudobulbus Bletillae (Rhizoma Bletillae) weight Times water, control water temperature for 50 DEG C of ultrasounds 2 hours, filter to get filtrate, the merging filtrate obtained by supersound process that adds water every time obtains second Filtrate;
First filtrate is removed into Sodium Chloride and water using dialysis, residue is collected and is dissolved in the second filtrate, and will Second filtrate is concentrated into 10 times that weight is Pseudobulbus Bletillae (Rhizoma Bletillae) weight.
Ethanol being added to the second filtrate after concentration and being mixed, the mass concentration for obtaining ethanol is 70% alcohol deposit fluid;By alcohol Heavy liquid standing sedimentation 12 hours, is collected by filtration precipitum and is dried, and obtains Bletilla glucomannan.
Embodiment 4
A kind of preparation method of Bletilla glucomannan, including:
The Pseudobulbus Bletillae (Rhizoma Bletillae) is wrapped up with plant ash, stirring uses the clean water Pseudobulbus Bletillae (Rhizoma Bletillae) after 20 minutes.
Under the conditions of 40 DEG C, the above-mentioned Pseudobulbus Bletillae (Rhizoma Bletillae) is soaked in into the ethanol solution 15min of the hydrochloric acid that mass concentration is 6%, is stirred; The floating thing for floating on liquid level is skimmed, the Pseudobulbus Bletillae (Rhizoma Bletillae) is pulled out and is used clean water.
The clean Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity for 50 mesh.
During the Pseudobulbus Bletillae (Rhizoma Bletillae) after crushing is added into weight for 5 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight of saturated nacl aqueous solution, mix and stand 8 points Clock;The floating thing for floating on liquid level is skimmed, the first filtering residue and the first filtrate is filtered to obtain.
By the first filtering residue weight is Pseudobulbus Bletillae (Rhizoma Bletillae) weight, 1.5 times of water soaks 5 hours, to immersion after the first filtering residue carry out 3 supersound process that add water, the supersound process that adds water is carried out in the following manner:Weight is added in the first filtrate for the 8 of Pseudobulbus Bletillae (Rhizoma Bletillae) weight Times water, control water temperature for 40 DEG C of ultrasounds 1 hour, filter to get filtrate, the merging filtrate obtained by supersound process that adds water every time obtains second Filtrate.
First filtrate is removed into Sodium Chloride and water using dialysis, residue is collected and is dissolved in the second filtrate, and will Second filtrate is concentrated into 10 times that weight is Pseudobulbus Bletillae (Rhizoma Bletillae) weight.
Ethanol being added to the second filtrate after concentration and being mixed, the mass concentration for obtaining ethanol is 70% alcohol deposit fluid;By alcohol Heavy liquid standing sedimentation 10 hours, is collected by filtration precipitum and is dried, and obtains Bletilla glucomannan.
Embodiment 5
A kind of preparation method of Bletilla glucomannan, including:
The Pseudobulbus Bletillae (Rhizoma Bletillae) is wrapped up with plant ash, stirring uses the clean water Pseudobulbus Bletillae (Rhizoma Bletillae) after 30 minutes.
Under the conditions of 50 DEG C, the above-mentioned Pseudobulbus Bletillae (Rhizoma Bletillae) is soaked in into the ethanol solution 20min of the hydrochloric acid that mass concentration is 8%, is stirred; The floating thing for floating on liquid level is skimmed, the Pseudobulbus Bletillae (Rhizoma Bletillae) is pulled out and is used clean water.
The clean Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity for 100 mesh.
During the Pseudobulbus Bletillae (Rhizoma Bletillae) after crushing is added into weight for 6 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight of saturated nacl aqueous solution, mix and stand 8 points Clock;The floating thing for floating on liquid level is skimmed, the first filtering residue and the first filtrate is filtered to obtain.
By the first filtering residue weight is Pseudobulbus Bletillae (Rhizoma Bletillae) weight, 2 times of water soaks 5 hours, to immersion after the first filtering residue carry out 3 The secondary supersound process that adds water, the supersound process that adds water is carried out in the following manner:Weight is added in the first filtrate for 8 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight Water, control water temperature for 40 DEG C of ultrasounds 1.5 hours, filter to get filtrate, the merging supersound process gained filtrate that adds water every time obtains second Filtrate.
First filtrate is removed into Sodium Chloride and water using dialysis, residue is collected and residue is dissolved in into the second filtrate, And it is 10 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight that the second filtrate is concentrated into into weight.
Ethanol being added to the second filtrate after concentration and being mixed, the mass concentration of ethanol is 60% alcohol deposit fluid;By alcohol Heavy liquid standing sedimentation 10 hours, is collected by filtration precipitum and is dried, and obtains Bletilla glucomannan.
Embodiment 6
A kind of preparation method of Bletilla glucomannan, including:
The Pseudobulbus Bletillae (Rhizoma Bletillae) is wrapped up with plant ash, stirring uses the clean water Pseudobulbus Bletillae (Rhizoma Bletillae) after 20 minutes.
Under the conditions of 40 DEG C, the above-mentioned Pseudobulbus Bletillae (Rhizoma Bletillae) is soaked in into the ethanol solution 15min of the hydrochloric acid that mass concentration is 6%, is stirred; The floating thing for floating on liquid level is skimmed, the Pseudobulbus Bletillae (Rhizoma Bletillae) is pulled out and is used clean water.
The clean Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity for 50 mesh.
During the Pseudobulbus Bletillae (Rhizoma Bletillae) after crushing is added into weight for 4 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight of saturated nacl aqueous solution, mix and stand 5 points Clock;The floating thing for floating on liquid level is skimmed, the first filtering residue and the first filtrate is filtered to obtain.
By the first filtering residue weight is Pseudobulbus Bletillae (Rhizoma Bletillae) weight, 2 times of water soaks 6 hours, to immersion after the first filtering residue carry out 3 The secondary supersound process that adds water, the supersound process that adds water is carried out in the following manner:Weight is added in the first filtrate for the 12 of Pseudobulbus Bletillae (Rhizoma Bletillae) weight Times water, control water temperature for 50 DEG C of ultrasounds 1.5 hours, filter to get filtrate, the merging filtrate obtained by supersound process that adds water every time obtains the Two filtrates.
First filtrate is removed into Sodium Chloride and water using dialysis, residue is collected and residue is dissolved in into the second filtrate, And it is 12 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight that the second filtrate is concentrated into into weight.
Ethanol being added to the second filtrate after concentration and being mixed, the mass concentration for obtaining ethanol is 70% alcohol deposit fluid;By alcohol Heavy liquid standing sedimentation 12 hours, is collected by filtration precipitum and is dried, and obtains Bletilla glucomannan.
Embodiment 7
A kind of preparation method of Bletilla glucomannan, including:
The Pseudobulbus Bletillae (Rhizoma Bletillae) is wrapped up with plant ash, stirring uses the clean water Pseudobulbus Bletillae (Rhizoma Bletillae) after 30 minutes.
Under the conditions of 50 DEG C, the above-mentioned Pseudobulbus Bletillae (Rhizoma Bletillae) is soaked in into the ethanol solution 15min of the hydrochloric acid that mass concentration is 8%, is stirred; The floating thing for floating on liquid level is skimmed, the Pseudobulbus Bletillae (Rhizoma Bletillae) is pulled out and is used clean water.
The clean Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity for 100 mesh.
During the Pseudobulbus Bletillae (Rhizoma Bletillae) after crushing is added into weight for 6 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight of saturated nacl aqueous solution, mix and stand 10 points Clock;The floating thing for floating on liquid level is skimmed, the first filtering residue and the first filtrate is filtered to obtain.
By the first filtering residue weight is Pseudobulbus Bletillae (Rhizoma Bletillae) weight, 2 times of water soaks 6 hours, to immersion after the first filtering residue carry out 2 The secondary supersound process that adds water, the supersound process that adds water is carried out in the following manner:Weight is added in the first filtrate for the 12 of Pseudobulbus Bletillae (Rhizoma Bletillae) weight Times water, control water temperature for 40 DEG C of ultrasounds 2 hours, filter to get filtrate, the merging filtrate obtained by supersound process that adds water every time obtains second Filtrate.
First filtrate is removed into Sodium Chloride and water using dialysis, residue is collected and residue is dissolved in into the second filtrate, And it is 10 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight that the second filtrate is concentrated into into weight.
Ethanol being added to the second filtrate after concentration and being mixed, the mass concentration for obtaining ethanol is 80% alcohol deposit fluid;By alcohol Heavy liquid standing sedimentation 12 hours, is collected by filtration precipitum and is dried, and obtains Bletilla glucomannan.
Embodiment 8
A kind of preparation method of Bletilla glucomannan, including:
The Pseudobulbus Bletillae (Rhizoma Bletillae) is wrapped up with plant ash, stirring uses the clean water Pseudobulbus Bletillae (Rhizoma Bletillae) after 20 minutes.
Under the conditions of 40 DEG C, the above-mentioned Pseudobulbus Bletillae (Rhizoma Bletillae) is soaked in into the ethanol solution 15min of the hydrochloric acid that mass concentration is 6%, is stirred; The floating thing for floating on liquid level is skimmed, the Pseudobulbus Bletillae (Rhizoma Bletillae) is pulled out and is used clean water.
The clean Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity for 50 mesh.
During the Pseudobulbus Bletillae (Rhizoma Bletillae) after crushing is added into weight for 6 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight of saturated nacl aqueous solution, mix and stand 8 points Clock;The floating thing for floating on liquid level is skimmed, the first filtering residue and the first filtrate is filtered to obtain.
By the first filtering residue weight is Pseudobulbus Bletillae (Rhizoma Bletillae) weight, 2 times of water soaks 5 hours, to immersion after the first filtering residue carry out 2 The secondary supersound process that adds water, the supersound process that adds water is carried out in the following manner:Weight is added in the first filtrate for the 12 of Pseudobulbus Bletillae (Rhizoma Bletillae) weight Times water, control water temperature for 40 DEG C of ultrasounds 1.5 hours, filter to get filtrate, the merging filtrate obtained by supersound process that adds water every time obtains the Two filtrates.
First filtrate is removed into Sodium Chloride and water using dialysis, residue is collected and residue is dissolved in into the second filtrate, And it is 10 times of Pseudobulbus Bletillae (Rhizoma Bletillae) weight that the second filtrate is concentrated into into weight;
Ethanol being added to the second filtrate after concentration and being mixed, the mass concentration for obtaining ethanol is 70% alcohol deposit fluid;By alcohol Heavy liquid standing sedimentation 10 hours, is collected by filtration precipitum and is dried, and obtains Bletilla glucomannan.
1. Bletilla glucomannan extraction ratio computing formula:Bletilla glucomannan extraction ratio=Bletilla glucomannan weight/Pseudobulbus Bletillae (Rhizoma Bletillae) medical material weight × 100%.
Precision weighs the weight of the Pseudobulbus Bletillae (Rhizoma Bletillae) raw material of embodiment 1-8 and the weight of obtained Bletilla glucomannan, by Bletilla glucomannan extraction ratio Computing formula is calculated the extraction ratio of the Bletilla glucomannan of embodiment 1-8, and its result is as shown in the table:
The extraction ratio of the Bletilla glucomannan of table 1.
It can be seen from table 1, the extraction ratio of the preparation method of Bletilla glucomannan its Bletilla glucomannan that embodiment 1-8 is provided is apparently higher than normal The extraction ratio of rule extraction method Bletilla glucomannan, and extraction ratio fluctuation is little.Illustrate that the preparation method of the Bletilla glucomannan that the present embodiment 1-8 is provided is high Imitate, stablize, extraction effect is substantially better than traditional extraction method.
2. the polyoses content of Bletilla glucomannan obtained in embodiment 1-8 is measured using Phenol-sulphate acid method, its result is as follows Shown in table:
The polyoses content of the Bletilla glucomannan of table 2.
Polysaccharide is used as the main active of Bletilla glucomannan, and its content is higher, and the drug effect of Bletilla glucomannan is higher.It can be seen from table 2, The preparation method of the Bletilla glucomannan that embodiment 1-8 is provided, the polyoses content of its Bletilla glucomannan for extracting is apparently higher than traditional extraction legal system The polyoses content of the Bletilla glucomannan for obtaining, and the Bletilla glucomannan polyoses content that each embodiment is extracted is close.Illustrate that embodiment 1-8 is provided white The preparation method extraction effect of splendid achnatherum glue is stablized, obtained Bletilla glucomannan good drug efficacy.
In sum, the extraction ratio of the preparation method Bletilla glucomannan of Bletilla glucomannan of the present invention is high, and raw material availability is high, obtained white Splendid achnatherum glue product cost is low, purity is high, Pseudobulbus Bletillae polysaccharose content high, pharmacological effect is good.
Embodiments described above is a part of embodiment of the invention, rather than the embodiment of whole.The reality of the present invention The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected enforcement of the present invention Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made Every other embodiment, belongs to the scope of protection of the invention.

Claims (10)

1. a kind of preparation method of Bletilla glucomannan, it is characterised in that include:
Pulverising step:The clean Pseudobulbus Bletillae (Rhizoma Bletillae) is crushed to into granularity for 10-100 mesh;
Screening step:The Pseudobulbus Bletillae (Rhizoma Bletillae) after by crushing adds the saturated nacl aqueous solution of 4-6 times that weight is the Pseudobulbus Bletillae (Rhizoma Bletillae) weight In, mix and stand 5-10 minutes;
The floating thing for floating on liquid level is skimmed, the first filtering residue and the first filtrate is filtered to obtain;
Extraction step:Added water at least one times supersound process to first filtering residue, every time it is described add water supersound process by with Under type is carried out:Addition weight is the water of 8-12 times of the Pseudobulbus Bletillae (Rhizoma Bletillae) weight in the first filtering residue, and ultrasonic 1-2 hours are filtered Filtrate, merges every time the filtrate added water obtained by supersound process and obtains the second filtrate;
Purification step:Ethanol is added to second filtrate and mix to obtain alcohol deposit fluid, the quality of ethanol described in the alcohol deposit fluid Concentration is 50%-80%;
By the alcohol deposit fluid standing sedimentation 8-12 hours, precipitum is collected by filtration and is dried, obtain the Bletilla glucomannan.
2. the preparation method of Bletilla glucomannan according to claim 1, it is characterised in that be also included in the purification step it Before, first filtrate is removed into Sodium Chloride and water using dialysis, collect residue and the residue is dissolved in into described the The step of two filtrate.
3. the preparation method of Bletilla glucomannan according to claim 1, it is characterised in that be also included in the pulverising step it Before, the Pseudobulbus Bletillae (Rhizoma Bletillae) is wrapped up with plant ash, the step of use clean water after stirring 10-30 minutes.
4. the preparation method of Bletilla glucomannan according to claim 1, it is characterised in that before being also included in the pulverising step Peeling step, the peeling step carries out in the following manner:
Under the conditions of 30 DEG C -50 DEG C, the Pseudobulbus Bletillae (Rhizoma Bletillae) is soaked in into the ethanol solution 10min- of the hydrochloric acid that mass concentration is 3%-8% 20min, stirring;
The floating thing for floating on liquid level is skimmed, the Pseudobulbus Bletillae (Rhizoma Bletillae) is pulled out and is used clean water.
5. the preparation method of Bletilla glucomannan according to claim 1, it is characterised in that be also included in the supersound process that adds water Before, by 1-2 times that the first filtering residue weight is the Pseudobulbus Bletillae (Rhizoma Bletillae) weight of water immersion 4-6 hours the step of.
6. the preparation method of Bletilla glucomannan according to claim 1, it is characterised in that it is described add water supersound process when water temperature be 30℃-50℃。
7. the preparation method of Bletilla glucomannan according to claim 1, it is characterised in that described to add water in the extraction step The number of times of supersound process is 1-3 time.
8. the preparation method of Bletilla glucomannan according to claim 1, it is characterised in that the matter of ethanol described in the alcohol deposit fluid Amount concentration is 60%-70%.
9. the preparation method of Bletilla glucomannan according to claim 1, it is characterised in that be also included in before purification step, will Second filtrate is concentrated into 8-12 times that weight is the Pseudobulbus Bletillae (Rhizoma Bletillae) weight.
10. a kind of Bletilla glucomannan, it is characterised in that the preparation method of the Bletilla glucomannan according to any one of claim 1-9 is obtained.
CN201710060316.3A 2017-01-24 2017-01-24 Bletilla striata gelatin and preparation method thereof Pending CN106674370A (en)

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CN109381449A (en) * 2018-10-24 2019-02-26 广西信业生物技术有限公司 A kind of dermatitis antibacterial film forming spray and preparation method thereof
CN115813837A (en) * 2022-11-28 2023-03-21 现代百朗德生物科技(江苏)有限公司 Bletilla striata hydrolyzed horse oil chilblain cream and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN107501434A (en) * 2017-09-29 2017-12-22 贵州同源中药发展有限公司 A kind of bletilla striata polyoses glue extracting method
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CN109381449A (en) * 2018-10-24 2019-02-26 广西信业生物技术有限公司 A kind of dermatitis antibacterial film forming spray and preparation method thereof
CN115813837A (en) * 2022-11-28 2023-03-21 现代百朗德生物科技(江苏)有限公司 Bletilla striata hydrolyzed horse oil chilblain cream and preparation method thereof

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Application publication date: 20170517