CN111548430A - Preparation method of dendrobe polysaccharide and product thereof - Google Patents
Preparation method of dendrobe polysaccharide and product thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of dendrobe polysaccharide, which comprises the following steps: s1, heating water to a preset temperature, putting dendrobium officinale sections into the water, and preserving heat; s2, squeezing the mixed liquor obtained in the step S1, and separating to obtain slag and squeezed liquor; s3, adding a calcium hydroxide solution into the squeezed liquid obtained in the step S2, filtering, and collecting filtrate; s4, decoloring the filtrate obtained in the step S3 to obtain the dendrobium polysaccharide. The preparation method has the advantages of simple process, easy filtration, no organic solvent, no enzyme, less solid waste and contribution to production amplification, and meanwhile, the invention has breakthrough in eliminating opalescence, improving yield and keeping long-term stability and is beneficial to production conversion and product application.
Description
Technical Field
The invention relates to the technical field of biomedicine and cosmetics, in particular to a preparation method of dendrobe polysaccharide and a product thereof.
Background
Dendrobium officinale is a traditional rare medicinal material, is listed in a list of homology of medicine and food at present, and is distinguished from other varieties of dendrobium in pharmacopoeia and is separately and purely contained, so that the dendrobium officinale has profound significance for development of dendrobium officinale. In the technical field of biological medicines, modern pharmacological studies prove that the main active component in the dendrobium officinale is dendrobium polysaccharide, and the dendrobium officinale polysaccharide has various biological functions of reducing blood fat, reducing blood sugar, resisting tumors, improving immunity and the like. In the technical field of cosmetics, dendrobium polysaccharide is also increasingly reused, and particularly has good effects in the aspects of moisturizing, anti-allergy, anti-inflammation, anti-aging, skin repair and the like.
According to the traditional extraction method of the dendrobium polysaccharide, the dry dendrobium is used as a raw material, the process is complex, the extraction rate is low, solid-liquid separation is difficult, in order to improve the yield, cellulase or alkaline water is mostly adopted to destroy the cell wall, and the enzyme or the alkaline is used to destroy part of the dendrobium polysaccharide while destroying the cell wall. Chinese patent CN201710654381.9 discloses a process for preparing dendrobium candidum polysaccharide by an enzyme method, wherein pectinase is used for hydrolyzing pectin, so that the viscosity is reduced, and the problem of difficult filtration is solved; cellulose is hydrolyzed by using cellulase, so that the dissolution of polysaccharide is facilitated; the laccase is used for oxidizing polyphenol to improve stability, however, although the enzyme has high efficiency and specificity, the industrial enzyme can hydrolyze dendrobium polysaccharide very quickly, so that the yield is influenced, and the risk is brought to the stability of the process.
At present, the method for extracting dendrobium polysaccharides by using fresh dendrobium is less, for example, Chinese patent CN201610766175.2 discloses dendrobium polysaccharides and a preparation method and application thereof, wherein a method for extracting the dendrobium polysaccharides after crushing and pulping fresh raw materials is described, however, the crushing and pulping can cause fine fibers, the viscosity of slurry is high, the difficulty of solid-liquid separation is increased, and the large-scale production is difficult to realize.
Activated carbon is mostly needed for decolorization of dendrobium polysaccharides at the present stage, but activated carbon has no selectivity on adsorption of polysaccharides and adsorption of pigments, a large amount of polysaccharides are adsorbed while pigments are adsorbed, so that the extraction rate is low, and in addition, a patent is also provided for methylating polyphenol by adding laccase to solve the problem of color change formed after the oxidation of polyphenol, such as Chinese patent CN 201710654381.9.
In addition, the thickening effect of the carbomer thickening agent is reduced due to the salt content in the extracted dendrobium polysaccharide, so that the quality of downstream products cannot be guaranteed, and most of dendrobium polysaccharide is not paid attention to the thickening effect in production.
Disclosure of Invention
In order to solve the above problems, the first aspect of the present invention provides a method for preparing dendrobe polysaccharide, comprising the following steps:
s1, heating water to a preset temperature, putting dendrobium officinale sections into the water, and preserving heat;
s2, squeezing the mixed liquor obtained in the step S1, and separating to obtain slag and squeezed liquor;
s3, adding a calcium hydroxide solution into the squeezed liquid obtained in the step S2, filtering, and collecting filtrate;
s4, decoloring the filtrate obtained in the step S3 to obtain the dendrobium polysaccharide.
As a preferred technical scheme, the dendrobium officinale sections are obtained by cutting fresh dendrobium officinale into sections.
As a preferable technical solution, the step S2 further includes secondary pressing of the slag; the secondary pressing of the slag comprises the following steps: adding the residues into water, heating to a preset temperature, preserving heat, squeezing, and combining squeezed liquids obtained by squeezing twice.
As a preferable technical scheme, the filtrate is decolorized in the step S4 by using snake cage resin.
As a preferred technical solution, the step S4 further includes desalting.
As an optimal technical scheme, the length of the dendrobium officinale sections is 0.5-1.5 cm.
As a preferred technical scheme, the preset temperature is 85-95 ℃.
As a preferable technical scheme, the heat preservation time in the step S1 is 1.5-3 h.
As a preferable technical scheme, the heat preservation time in the secondary pressing is 0.5-1.5 h.
The second aspect of the invention provides dendrobe polysaccharide, which is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts the method of fresh branch cutting, enzyme deactivation and squeezing, eliminates the hydrolysis of endogenous enzyme on polysaccharide by using high temperature, improves the yield of polysaccharide, reduces the viscosity of the dendrobium extract, and is beneficial to accelerating the slag-liquid separation in the squeezing process; the fresh dendrobium is cut into small sections, so that the contact area of the dendrobium and water is increased, the extraction speed is increased, and the separation speed of the residue liquid extract after rear-end pressing is not influenced; water is added for extraction twice, so that the concentration of the dendrobium polysaccharide in the residues is diluted, and the residue of the dendrobium polysaccharide in the residues is reduced; the residue and the liquid can be quickly and fully separated by twice squeezing, and the residue of the dendrobium polysaccharide in the residue is reduced, so that the polysaccharide is effectively extracted, the extraction speed is high, and the extraction time is short;
(2) the invention effectively extracts pectin, polyphenol, acidic protein, starch and other substances in the solution by using a saturated limewater complexing precipitation method, namely, the effective content of polysaccharide is increased, so that the stability of the dendrobium polysaccharide is greatly improved, and the dendrobium polysaccharide can be stably applied to biological medicines, health products, foods and cosmetics, particularly liquid products and salt-resistant carbomer thickening products;
(3) the preparation method disclosed by the invention is easy to filter in the process of producing the dendrobium polysaccharide, simple in process steps, beneficial to large-scale production, free of organic solvent in the whole preparation process, more environment-friendly and in line with the standards of solvent residues of medicines, health products, foods and cosmetics; in addition, no enzyme is used in the process, the cost is controlled, and the production efficiency and the polysaccharide yield are improved;
(4) the preparation method of the invention has breakthrough in removing opalescence, improving yield and keeping long-term stability of the solution, and is beneficial to production conversion and application of downstream products.
Detailed Description
The invention will be further understood by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.
As used herein, a feature that does not define a singular or plural form is also intended to include a plural form of the feature unless the context clearly indicates otherwise. It will be further understood that the term "prepared from …," as used herein, is synonymous with "comprising," including, "comprising," "having," "including," and/or "containing," when used in this specification means that the recited composition, step, method, article, or device is present, but does not preclude the presence or addition of one or more other compositions, steps, methods, articles, or devices. Furthermore, the use of "preferred," "preferably," "more preferred," etc., when describing embodiments of the present application, is meant to refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. In addition, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
In order to solve the above problems, the first aspect of the present invention provides a method for preparing dendrobe polysaccharide, comprising the following steps:
s1, heating water to a preset temperature, putting dendrobium officinale sections into the water, and preserving heat;
s2, squeezing the mixed liquor obtained in the step S1, and separating to obtain slag and squeezed liquor;
s3, adding a calcium hydroxide solution into the squeezed liquid obtained in the step S2, filtering, and collecting filtrate;
s4, decoloring the filtrate obtained in the step S3 to obtain the dendrobium polysaccharide.
In some preferred embodiments, the dendrobium officinale sections are obtained by cutting fresh dendrobium officinale into sections; preferably, the length of the dendrobium officinale sections is 0.5-1.5 cm.
The term "Dendrobium officinale" as used herein, having the scientific name Dendrobium officinale Kimura et Migo, an Orchidaceae herb. The term "dendrobium officinale segment" herein refers to a segment obtained by cutting off the stem of dendrobium officinale. The term "fresh dendrobium officinale" herein refers to the non-deteriorated dendrobium officinale which has been picked in a short period of time without drying treatment.
At present, the dried dendrobium officinale is used as a raw material for preparing most of dendrobium polysaccharides, large-scale equipment is usually needed for drying, the production cost of the dendrobium polysaccharides is increased, and in the drying process, the dendrobium polysaccharides can be degraded under the action of endogenous enzymes of the dendrobium officinale, so that the extraction rate is influenced.
The dendrobe polysaccharide is extracellular polysaccharide, is viscous liquid formed by pectin, starch, protein and O-acetylglucosamine in a mucous membrane cavity of dendrobe branches, is poor in fluidity, dry raw materials are generally crushed for improving the extraction yield, fresh raw materials are mostly pulped or homogenized for improving the yield to a certain extent, but the yield can be improved to a certain extent by adopting the modes, but the system viscosity is high, the separation of slag and liquid is difficult, the process difficulty is high, if the system viscosity needs to be reduced, a large amount of water needs to be used for dilution, concentration equipment is used for concentration after extraction is finished, and finally high-concentration dendrobe polysaccharide is obtained.
The inventor finds that the yield can be obviously improved by adopting the method for squeezing the fresh dendrobium officinale sections at high temperature, the process is greatly simplified, the energy is saved, and the cost is reduced, because the interaction between dendrobium polysaccharides and between the dendrobium polysaccharides and water molecules is weakened due to the high temperature, the mobility of the dendrobium polysaccharides is increased, the viscosity of the dendrobium extracting solution is reduced, and the method is favorable for accelerating the slag-liquid separation in the squeezing process; the high temperature can also inactivate endogenous enzymes, eliminate the hydrolysis of the endogenous enzymes on the polysaccharide and improve the yield of the polysaccharide.
The inventor finds that the length of the dendrobium officinale section is controlled within the optimal range, the extraction speed can be further accelerated, and the yield is improved, the reason is that the contact area of the dendrobium officinale section cut into small sections with water is increased, the dissolution of polysaccharide is promoted, the dissolution rate is within the controllable range, the problem that the viscosity of a system is increased too fast due to excessive polysaccharide in water is avoided, and the slag-liquid separation speed in subsequent squeezing is guaranteed.
When the dendrobium officinale cut into small segments is adopted as the raw material, the dissolution rate of the polysaccharide is controlled, so that the overhigh viscosity of the system is avoided, however, the dendrobium officinale residue after pressing can still have a part of dendrobium polysaccharide, and in some preferred embodiments, the step S2 further comprises secondary pressing of the residue from the viewpoint of improving the utilization rate of the raw material; the secondary pressing of the slag comprises the following steps: adding the residues into water, heating to a preset temperature, preserving heat, squeezing, and combining squeezed liquids obtained by squeezing twice.
The inventor unexpectedly discovers that twice squeezing has higher efficiency than once squeezing under the condition of achieving the same yield because the once extraction of the dendrobium polysaccharide with the same content can cause the viscosity of the system to be overlarge, the time for separating the slag and the liquid is longer, the efficiency is reduced, partial polysaccharide remains in the slag, the extraction is carried out twice, the concentration of the dendrobium polysaccharide in the slag and in water is diluted, the viscosity of the system is moderate, the slag and the liquid are easy to separate, the loss of the polysaccharide is reduced, the integral production efficiency is improved, and the large-scale production is facilitated.
From the viewpoint of adjusting the dissolution rate of the polysaccharide and reducing the hydrolysis of the polysaccharide, in some preferred embodiments, the preset temperature is 85 to 95 ℃; the heat preservation time in the step S1 is 1.5-3 h; and the heat preservation time in the secondary squeezing is 0.5-1.5 h.
From the viewpoint of improving the slag-liquid separation efficiency, in some preferred embodiments, the amount of water used in step S1 is 2-3.5 times the weight of the dendrobium officinale sections; the amount of water used in the secondary pressing is 0.5-4 times of the weight of the slag.
The term "calcium hydroxide solution" herein is also referred to as lime water. In some preferred embodiments, the calcium hydroxide solution is saturated lime water. The term "saturated lime water" herein refers to a saturated aqueous solution of calcium hydroxide.
In some preferred embodiments, the amount of the saturated limewater is 1-13 wt% of the dendrobium officinale sections.
The dendrobium polysaccharide extracted in the prior art is mostly a mixture formed by O-acetylglucosamine, pectin and alkaline protein, has high viscosity and is difficult to filter, certain difficulty is caused to production, and the produced solution is easy to opalescence, easy to discolor and precipitate after being placed for a long time, and is not beneficial to product storage and application. At present, in the process of preparing the dendrobium polysaccharide, substances such as starch, pectin and the like are removed by a multi-purpose enzyme method, but simultaneously, a large amount of dendrobium polysaccharide can be hydrolyzed, so that the yield of the dendrobium polysaccharide is reduced. The inventor finds that the efficiency of removing starch and pectin by using calcium hydroxide is higher and the product quality can be improved, and the reason is that calcium ions in the calcium hydroxide can be complexed with active groups such as hydroxyl, carboxyl and the like, pectin originally dispersed in all places of a system is gathered around the calcium ions to form a net structure, the starch is also interacted with the net structure to be coagulated to form precipitates, the viscosity of an extracting solution is greatly reduced, opalescence of the solution caused by substances such as pectin is eliminated, in addition, hydroxyl ions introduced by lime water can neutralize partial acidic protein, the calcium ions can flocculate the protein, the dendrobium polysaccharide is prevented from deteriorating in the storage process, and the shelf life of the product is prolonged.
In some preferred embodiments, the filtrate decolorization in step S4 uses a snake cage resin.
The term "snake cage resin", also known as snake cage polyelectrolyte or delayed ion exchange resin, as used herein, refers to a particular type of ion exchange resin containing a linear polymer with oppositely charged functional groups physically entrapped in a cross-linked polymer having specific charge exchange functional groups.
In some preferred embodiments, the snake cage resin is a strong acid weak base snake cage resin or a strong base weak acid snake cage resin.
The specific type of the snake cage resin used for decoloring in the present application is not particularly limited, and the snake cage resin is classified according to the parent resin skeleton of the cage, and examples thereof include snake cage resin using styrene strongly basic anion exchange resin as the cage, snake cage resin using styrene weakly basic anion exchange resin as the cage, snake cage resin using weakly basic epoxy anion exchange resin as the cage, snake cage resin using styrene strongly acidic cation exchange resin as the cage, and snake cage resin using acrylic weakly acidic cation exchange resin as the cage; as the homo-or copolymer of acrylic acid (ester) monomers, there may be mentioned, for example, snake cage resins of snake, snake cage resins of polypropylenephthalic amines, snake cage resins of snake, and snake cage resins of phenol-formaldehyde type cationic resin monomers, which are classified according to the chain structure of snake.
In some preferred embodiments, the decolorizing comprises the steps of: adjusting the pH value of the filtrate to 4.7-4.9, adding snake cage resin, decoloring for 0.5-1.5 h, filtering, and collecting the decolored dendrobe polysaccharide solution.
The agent for adjusting pH in the present application may be any known to those skilled in the art, such as acetic acid, citric acid, hydrochloric acid, and the like.
In some preferred embodiments, the snake cage resin is added in an amount of 1 to 5 wt% of the filtrate.
In the preparation process of the dendrobium polysaccharide, activated carbon is usually used for decoloring, and a large amount of dendrobium polysaccharide is adsorbed while adsorbing pigments, so that the yield is reduced. According to the invention, the snake cage resin is used for adsorbing charged pigments in the dendrobium polysaccharide, and simultaneously, the adsorption to the polysaccharide is not generated, so that the yield of the dendrobium polysaccharide is improved, the dendrobium polysaccharide solution is clear and bright, and the snake cage resin can be recycled after being washed by water, so that the discharge of solid waste and the pollution to the environment are reduced; in addition, the snake cage resin can also separate strong electrolyte in the solution, reduce the salt content in the solution and facilitate the development and production of downstream products.
In some preferred embodiments, the step S4 further comprises desalting.
The term "desalination" as used herein refers to the removal of chemical salts from a solution, i.e., the removal of anions and cations from water.
The method of desalination in this application may be any known to those skilled in the art, such as ion exchange, or desalination using commercially available reverse osmosis membrane equipment.
The inventor finds that the compatibility of the product with additives such as a surfactant, a thickening agent and the like is improved by desalting the dendrobium polysaccharide solution, and the application of the product in downstream products is facilitated.
The second aspect of the invention provides dendrobe polysaccharide, which is prepared by the preparation method.
Examples
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
Embodiment 1 provides a preparation method of dendrobe polysaccharide, comprising the following steps:
(1) weighing 50kg of fresh dendrobium officinale, and cutting into dendrobium officinale sections with the length of 0.8cm by using a cutting machine;
(2) weighing 150kg of water, adding the water into an extraction tank, and heating to 85 ℃; then adding the dendrobium officinale processed in the step (1), inactivating enzyme at 85 ℃ and extracting for 1.5 hours;
(3) squeezing the mixed solution obtained in the step (2) to obtain 175kg of squeezed solution, and the balance being slag;
(4) adding 50kg of water into the slag obtained in the step (3), extracting at 85 ℃ for 1 hour, and squeezing again to obtain 55kg of squeezed liquid;
(5) mixing the squeezed solutions obtained in the steps (3) and (4), adding 5kg of saturated lime water, stirring and reacting for 30min, and filtering by using a plate frame to obtain 230kg of filtrate;
(6) adjusting the pH of the filtrate obtained in the step (5) to 4.8, adding 3kg of strong acid weak base type snake cage resin, decoloring for 1h, and filtering with a plate frame to obtain 225kg of dendrobium polysaccharide solution;
(7) and (4) desalting and deacidifying the solution obtained in the step (6) by using reverse osmosis membrane equipment to obtain 220kg of clear and transparent dendrobium polysaccharide solution.
Example 2
Embodiment 2 provides a preparation method of dendrobe polysaccharide, comprising the following steps:
(1) weighing 100kg of dendrobium officinale, and cutting into dendrobium officinale sections with the length of 0.5cm by using a cutting machine;
(2) weighing 320kg of water, adding the water into an extraction tank, and heating to 90 ℃; then adding the dendrobium officinale processed in the step (1), inactivating enzyme at 90 ℃ and extracting for 1.5 hours;
(3) squeezing the mixed liquid obtained in the step (2) to obtain 375kg of filtrate, and the balance being slag;
(4) adding 150kg of water into the slag obtained in the step (3), extracting for 1 hour at 90 ℃, and squeezing again to obtain 155kg of squeezed liquid;
(5) mixing the filtrates in the steps (3) and (4), adding 12kg of saturated lime water, stirring and reacting for 30min, and filtering by a plate frame to obtain 532kg of liquid;
(6) adjusting the pH of the filtrate obtained in the step (5) to 4.75, adding 8kg of strong acid weak base type snake cage resin, decoloring for 1h, and filtering with a plate frame to obtain 491kg of dendrobe polysaccharide solution;
(7) and (4) desalting and deacidifying the solution obtained in the step (6) by using reverse osmosis membrane equipment to obtain 488kg of clear and transparent dendrobium polysaccharide solution.
Example 3
Embodiment 3 provides a method for preparing dendrobium polysaccharides, comprising the following steps:
(1) weighing 200kg of dendrobium officinale, and cutting into dendrobium officinale sections with the length of 1.4cm by using a cutting machine;
(2) weighing 500kg of water, adding the water into an extraction tank, and heating to 95 ℃; then adding the dendrobium officinale processed in the step (1), inactivating enzyme at 95 ℃ and extracting for 1.5 hours;
(3) squeezing the mixed liquid obtained in the step (2) to obtain 600kg of squeezed liquid, and the balance being slag;
(4) adding 400kg of water into the slag obtained in the step (3), extracting at 95 ℃ for 1 hour, and squeezing again to obtain 415kg of filtrate;
(5) mixing the squeezed liquids in the steps (3) and (4), adding 25kg of saturated lime water, stirring and reacting for 30min, and filtering by using a plate frame to obtain 1010kg of liquid;
(6) adjusting the pH of the filtrate obtained in the step (5) to 4.85, adding 30kg of strong acid weak base type snake cage resin, decoloring for 1h, and filtering with a plate frame to obtain 1000kg of dendrobium polysaccharide solution;
(7) and (4) desalting and deacidifying the solution obtained in the step (6) by using reverse osmosis membrane equipment to obtain 995kg of clear and transparent dendrobium polysaccharide solution.
Comparative example 1
Comparative example 1 provides a method for preparing dendrobium polysaccharides, comprising the following steps:
(1) weighing 50kg of fresh dendrobium officinale, adding 150kg of water, and pulping to obtain pulp;
(2) heating the slurry obtained in the step (1) to 85 ℃ to inactivate enzyme and extracting for 1.5 hours;
(3) performing plate-frame filtration on the mixed solution obtained in the step (2) to obtain 145kg of filtrate, and the balance being slag;
(4) adding 50kg of water into the slag obtained in the step (3), extracting for 1 hour at 85 ℃, and filtering by using a plate frame again to obtain 55kg of filtrate;
(5) mixing the filtrates in the steps (3) and (4), adding 5kg of saturated lime water, stirring and reacting for 30min, and filtering by a plate frame to obtain 230kg of filtrate;
(6) adjusting the pH of the filtrate obtained in the step (5) to 4.8, adding 3kg of strong acid weak base type snake cage resin, decoloring for 1h, and filtering with a plate frame to obtain 225kg of dendrobium polysaccharide solution;
(7) and (4) desalting and deacidifying the solution obtained in the step (6) by using reverse osmosis membrane equipment to obtain 220kg of clear and transparent dendrobium polysaccharide solution.
Comparative example 2
Comparative example 2 provides a method for preparing dendrobium polysaccharides, comprising the following steps:
(1) weighing 50kg of fresh dendrobium officinale, and cutting into dendrobium officinale sections with the length of 0.8cm by using a cutting machine;
(2) weighing 150kg of water, adding the water into an extraction tank, and heating to 85 ℃; then adding the dendrobium officinale processed in the step (1), inactivating enzyme at 85 ℃ and extracting for 1.5 hours;
(3) squeezing the mixed solution obtained in the step (2) to obtain 175kg of squeezed solution, and the balance being slag;
(4) adding 50kg of water into the slag obtained in the step (3), extracting at 85 ℃ for 1 hour, and squeezing again to obtain 55kg of squeezed liquid;
(5) combining the squeezed solutions in the steps (3) and (4), adjusting the pH to 4.8, adding 3kg of strong acid weak base type snake cage resin, decoloring for 1h, and filtering with a plate frame to obtain 225kg of dendrobe polysaccharide solution;
(6) and (5) desalting and deacidifying the solution obtained in the step (5) by using reverse osmosis membrane equipment to obtain 220kg of clear and transparent dendrobium polysaccharide solution.
Comparative example 3
Comparative example 3 provides a method for preparing dendrobium polysaccharides, comprising the following steps:
(1) weighing 50kg of fresh dendrobium officinale, and cutting into dendrobium officinale sections with the length of 0.8cm by using a cutting machine;
(2) weighing 150kg of water, adding the water into an extraction tank, and heating to 85 ℃; then adding the dendrobium officinale processed in the step (1), inactivating enzyme at 85 ℃ and extracting for 1.5 hours;
(3) squeezing the mixed solution obtained in the step (2) to obtain 175kg of squeezed solution, and the balance being slag;
(4) adding 50kg of water into the slag obtained in the step (3), extracting at 85 ℃ for 1 hour, and squeezing again to obtain 55kg of squeezed liquid;
(5) mixing the squeezed solutions obtained in the steps (3) and (4), adding 5kg of saturated lime water, stirring and reacting for 30min, and filtering by using a plate frame to obtain 230kg of filtrate;
(7) and (5) desalting and deacidifying the filtrate obtained in the step (5) by using reverse osmosis membrane equipment to obtain 220kg of clear and transparent dendrobium polysaccharide solution.
Comparative example 4
Embodiment 1 provides a preparation method of dendrobe polysaccharide, comprising the following steps:
(1) weighing 50kg of fresh dendrobium officinale, and cutting into dendrobium officinale sections with the length of 0.8cm by using a cutting machine;
(2) weighing 150kg of water, adding the water into an extraction tank, and heating to 85 ℃; then adding the dendrobium officinale processed in the step (1), inactivating enzyme at 85 ℃ and extracting for 1.5 hours;
(3) squeezing the mixed solution obtained in the step (2) to obtain 175kg of squeezed solution, and the balance being slag;
(4) adding 50kg of water into the slag obtained in the step (3), extracting at 85 ℃ for 1 hour, and squeezing again to obtain 55kg of squeezed liquid;
(5) mixing the squeezed solutions in the steps (3) and (4), adjusting the pH to 4.8, heating to 40 ℃, adding 0.5kg of complex enzyme (the weight ratio of pectinase to cellulase to laccase is 1: 3: 2.5), stirring for reaction for 2h, and filtering by a plate frame to obtain 230kg of filtrate;
(6) adjusting the pH of the filtrate obtained in the step (5) to 4.8, adding 3kg of strong acid weak base type snake cage resin, decoloring for 1h, and filtering with a plate frame to obtain 225kg of dendrobium polysaccharide solution;
(7) and (4) desalting and deacidifying the solution obtained in the step (6) by using reverse osmosis membrane equipment to obtain 220kg of clear and transparent dendrobium polysaccharide solution.
Evaluation of Performance
And (3) performing analysis tests on the dendrobium polysaccharides obtained in the examples 1-3 and the comparative examples 1-4, wherein the test contents comprise the yield, the filtering difficulty, the opalescence effect and the stability of the dendrobium polysaccharides.
1. Yield of dendrobe polysaccharide: the test is carried out according to the content determination of polysaccharide under the item of 'dendrobium officinale' in the first part of 'Chinese pharmacopoeia' 2015 edition, and the yield is calculated according to the formula:
wherein m1 is the weight of the dendrobium polysaccharide solution, c1 is the content of total sugar in the dendrobium polysaccharide solution, m2 is the weight of dendrobium officinale, c2 is the content of total sugar in the dendrobium officinale, and the results are shown in table 1.
2. The filtration difficulty is as follows: see table 1, where more "+" indicates more difficult filtration.
3. And (3) opalescence effect: the clarity of the dendrobium polysaccharide solution was visually observed for judgment, and the results are shown in table 1.
4. Stability: the dendrobium polysaccharide solution of the embodiment 1-3 is stored for three months at the temperature of 45 ℃ and 4 ℃ and normal temperature, no color change and no precipitation are caused, and the precipitates of the comparative examples 2 and 3 are generated within 3-4 weeks at the temperature of 45 ℃ and 4 ℃.
TABLE 1
| Clarity of the product | Colour(s) | Yield of | Degree of difficulty of filtration | |
| Example 1 | Clear and transparent | Almost colorless | 85.5％ | + |
| Example 2 | Clear and transparent | Almost colorless | 87.3％ | + |
| Example 3 | Clear and transparent | Almost colorless | 84.1％ | + |
| Comparative example 1 | Clear and transparent | Almost colorless | 73.6％ | Step 3, filtration: ++++ |
| Comparative example 2 | Opalescence | Red colour | 86.5％ | Step 5, filtration: +++++ |
| Comparative example 3 | Faint opalescence | Yellow colour | 88.3％ | + |
| Comparative example 4 | Clear and transparent | Almost colorless | 65.2％ | ++ |
According to the embodiments 1-3 and the comparative examples 1-4, the preparation method of the dendrobium polysaccharide provided by the invention has the advantages that the dendrobium polysaccharide does not need to be dried, the process is simple, the yield of the polysaccharide is high, the quality is high, a large amount of water resources and energy can be saved in the preparation process, and the preparation method is suitable for being widely popularized in the industry.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. The preparation method of the dendrobium polysaccharide is characterized by comprising the following steps:
s1, heating water to a preset temperature, putting dendrobium officinale sections into the water, and preserving heat;
s2, squeezing the mixed liquor obtained in the step S1, and separating to obtain slag and squeezed liquor;
s3, adding a calcium hydroxide solution into the squeezed liquid obtained in the step S2, filtering, and collecting filtrate;
s4, decoloring the filtrate obtained in the step S3 to obtain the dendrobium polysaccharide.
2. The method for preparing the dendrobium polysaccharide of claim 1, wherein the dendrobium officinale sections are obtained by cutting fresh dendrobium officinale into sections.
3. The method for preparing dendrobium polysaccharides of claim 1, wherein the step S2 further comprises secondary pressing of the residue; the secondary pressing of the slag comprises the following steps: adding the residues into water, heating to a preset temperature, preserving heat, squeezing, and combining squeezed liquids obtained by squeezing twice.
4. The method for preparing dendrobium polysaccharides in claim 1, wherein snake cage resin is used for decoloring the filtrate in the step S4.
5. The method for preparing dendrobe polysaccharide of claim 1, wherein step S4 further comprises desalting.
6. The method for preparing dendrobium polysaccharides of claim 1 or 2, wherein the length of the dendrobium officinale sections is 0.5-1.5 cm.
7. The method for preparing dendrobium polysaccharides of claim 1 or 3, wherein the preset temperature is 85-95 ℃.
8. The preparation method of dendrobe polysaccharide of claim 1, wherein the heat preservation time in step S1 is 1.5-3 h.
9. The preparation method of dendrobe polysaccharide as claimed in claim 3, wherein the heat preservation time in the secondary pressing is 0.5-1.5 h.
10. Dendrobe polysaccharide, which is characterized by being prepared by the preparation method of any one of claims 1 to 9.
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| CN113388048A (en) * | 2021-07-08 | 2021-09-14 | 晨光生物科技集团股份有限公司 | Preparation method of high-purity garlic polysaccharide |
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| CN113388048A (en) * | 2021-07-08 | 2021-09-14 | 晨光生物科技集团股份有限公司 | Preparation method of high-purity garlic polysaccharide |
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Application publication date: 20200818 |