CN108164572B - Method for extracting tannic acid by using dendrobe - Google Patents
Method for extracting tannic acid by using dendrobe Download PDFInfo
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- CN108164572B CN108164572B CN201810116619.7A CN201810116619A CN108164572B CN 108164572 B CN108164572 B CN 108164572B CN 201810116619 A CN201810116619 A CN 201810116619A CN 108164572 B CN108164572 B CN 108164572B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H13/00—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids
- C07H13/02—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids
- C07H13/08—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids having the esterifying carboxyl radicals directly attached to carbocyclic rings
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/60—Sugars; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
Abstract
The invention relates to the technical field of tannic acid extraction, and particularly relates to a method for extracting tannic acid by using dendrobe. The invention discloses a tannic acid extraction method, which selects any one or more than one of dendrobium huoshanense, dendrobium officinale, dendrobium cuprum, dendrobium loddigesii, dendrobium candidum, dendrobium loddigesii, dendrobium nobile and resin purification and other separation and purification technologies, effectively extracts tannic acid with excellent texture and pure white color, the purity of the finished product tannic acid is 94.7%, the extraction rate is 92.3%, the utilization rate and the utilization value of the dendrobium loddigesii are effectively improved, the extracted finished product tannic acid has obvious and strong effects in the fields of food, chemical industry, cosmetics, medicine and the like, and the medical effect of the same amount of tannic acid is 3-7% greater than that of the tannic acid extracted by schisandra chinensis.
Description
Technical Field
The invention relates to the technical field of tannic acid extraction, and particularly relates to a method for extracting tannic acid by using dendrobe.
Background
Dendrobium nobile also known as Hawthorn, chlorophytum comosum, Linlan, bansheng, and Taoist flower. The stem is upright, the meat is fleshy and thick, the stem is in a slightly flat cylindrical shape, the length of the stem is 10-60 cm, and the thickness of the stem reaches 1.3 cm. The dendrobium is a medicinal plant, has sweet, light and slightly salty taste and cold property, and enters stomach, kidney and lung channels. The dendrobium nobile has elegant, exquisite and lovely flowers, bright colors and aromatic smell, and is liked to be one of four ornamental foreign flowers.
Tannin, also called tannin and tannin, exists in barks and fruits of various trees, is also the main component of galls generated by insect attack on the trees, and the content can reach 50 to 70 percent. Tannin is yellow or brown yellow amorphous loose powder, has strong hygroscopicity, is insoluble in diethyl ether, benzene and chloroform, is easily soluble in water, ethanol and acetone, and has astringent taste in water solution. Tannins are not single compounds, and their chemical composition is complicated and can be roughly divided into two types, one is condensed tannins, flavanol derivatives, and the 2 nd position of flavonol in the molecule is bonded to catechol or benzenetriol through a C-C single bond. One is hydrolyzable tannin with ester bond in the molecule, and is gallic acid ester of glucose. Tannins have long been used only by our people to tanne hides and convert them into leather. Since the 50 s of the 20 th century, the activity of tannin capable of reacting with protein, polysaccharide, alkaloid, microorganism, enzyme and metal ion and the actions of antioxidation, free radical capturing, bacteriostasis and derivatization are revealed, and the application prospect and range of the tannin are rapidly expanded.
The existing tannin extraction raw materials are mainly schisandra chinensis, and the tannin content in the schisandra chinensis is 95-98%; however, the dendrobium also contains a large amount of tannin components, and the dendrobium is commonly called as pandas in the pharmaceutical industry, and has obvious and strong medicinal effect. Chinese patent 103910810A proposes a method for simultaneously preparing pigment and polysaccharide from herba Dendrobii, which draws the sequence of extracting effective components from herba Dendrobii, and extracts various effective components from herba Dendrobii by extraction, concentration, extraction, distillation, etc. in the existing processing technology, but the technology for extracting tannic acid from herba Dendrobii has not been reported yet.
Disclosure of Invention
In order to solve the problems, improve the utilization rate of the effective components of the dendrobium and enlarge the utilization range of the dendrobium, the invention provides a method for extracting tannic acid by using the dendrobium.
The invention is realized by the following technical scheme:
a method for extracting tannic acid by using dendrobe comprises the following steps:
a. cleaning a large amount of dendrobium stems with surface dust by using a brush, removing impurities, shearing into stem sections with the length of 4-5 cm, adding an organic hydrosolvent to completely immerse the dendrobium stems, and heating to 35 ℃ for soaking for 2-2.5 h;
b. adding an organic hydrosolvent which is 5-7 times of the stem of the dendrobium stem in weight part after soaking, heating in a water bath to 45-50 ℃, extracting at constant temperature for 8-10 h, filtering while hot, and taking a filtrate 1 for later use; adding organic hydrosolvent which is 7-8 times of the weight of the filter residue into the filter residue, heating the mixture in a water bath to 45-50 ℃, extracting the mixture for 5-6 hours at a constant temperature, filtering the mixture while the mixture is hot, taking a filtrate 2, and standing and draining the filter residue for later use;
c. mixing the filtrate 1 and the filtrate 2, stirring clockwise for 30s, stirring anticlockwise for 1min, concentrating at normal temperature and normal pressure to 1/5 of the original volume, then heating up and distilling at normal pressure, drying distillation residues at 62-65 ℃ in vacuum to obtain grey powder, crushing the grey powder, sieving the crushed grey powder with a 350-mesh sieve, crushing the sieved powder again, and sieving the crushed powder to obtain a coarse product tannin;
d. and (4) purifying the crude tannin.
Preferably, the dendrobium comprises one or more of dendrobium huoshanense, dendrobium officinale, dendrobium moniliforme, dendrobium loddigesii, dendrobium fimbriatum, dendrobium nobile and dendrobium nobile.
Preferably, the organic water solvent is a mixture of acetone, methanol and water, and the dosage ratio of the acetone, the methanol and the water is 1:1: 1.
Preferably, the methanol is 95% laboratory methanol and the acetone is 99.5% pure.
Preferably, in the step (c), the normal-pressure heating distillation pressure is 101.5kpa, the heating distillation temperature is 55-65 ℃, and the heating distillation is carried out until the organic solvent in the mixed filtrate is completely volatilized completely.
Preferably, the normal-pressure heating distillation operation is carried out in a fume hood, and the distillation device is provided with a condensation pipe and a tail gas recovery device;
in the process of normal-pressure heating distillation, the temperature is firstly increased from the initial temperature of the concentrated solution to 57 ℃ at the heating rate of 5 ℃/min, the temperature is kept constant, and the concentrated solution is distilled until no distillate is discharged;
then heating to 65 ℃ at the heating rate of 3 ℃/min, keeping the temperature constant, and ending the distillation until no distillate is distilled out.
Preferably, in step (b), the processing method of the filter residue for standby use is as follows:
adding 8 times of distilled water by weight into the standby filter residue, heating to 45 ℃, soaking for 12-14 h, uniformly stirring once every 35min, filtering after soaking, adding 10 times of well water by weight into the filtrate, adding 2% of monopotassium phosphate by weight of the filtrate, uniformly stirring and dissolving, and preparing the water soluble fertilizer for spraying and irrigating the dendrobium.
Preferably, the method for purifying the crude tannin comprises the following steps:
adding 2-3 times of distilled water by weight into the crude tannin, heating to 60 ℃ at a heating rate of 3 ℃/min, and stirring for dissolving for 30-35 min;
standing for 3min after uniform dissolution, quickly freezing in a freezing chamber at the temperature of 1-3 ℃, refrigerating for 24-25 h, taking out, standing to room temperature, and filtering to obtain a filtrate;
slowly filling the filtrate into AB-8 type large-aperture adsorption resin, loading the filtrate on a column at a rate of 7ml/s, eluting by using 1 time of distilled water by weight of the filtrate after the loading on the column is finished, and then eluting by using 3 times of 95% methanol solution by weight;
the elution was started with 1ml of 1% FeCl3Collecting the eluent in a 500ml big beaker, quickly replacing the beaker with a 1-5L transparent glass collecting device when purple precipitate appears in the beaker, and collecting the eluent;
and after adsorption and elution are finished, distilling the eluent collected by washing under normal pressure until the solvent is completely distilled, taking the residue, drying in vacuum at the temperature of 65-68 ℃, crushing and sieving with a 350-mesh sieve, crushing the part above the sieve again, and sieving to obtain the part below the sieve, namely the finished product tannin.
Preferably, the eluent atmospheric distillation method comprises the following steps:
the distillation pressure is 101.5kpa, the temperature is firstly increased to 57 ℃ from the initial temperature of the eluent according to the temperature rising rate of 5 ℃/min, the temperature is kept constant, and the distillation is carried out until no distillate is discharged;
then heating to 100 ℃ at the heating rate of 8 ℃/min, keeping the temperature constant, and ending the distillation when the distillate is not distilled out.
In the technical scheme provided by the invention, the finished product tannic acid is mainly applied to the field of medicine and is used for clinical medical treatment such as protecting arterial walls, preventing arteriosclerosis, regulating cholesterol, inhibiting platelet coagulation, preventing thrombus, protecting heart blood vessels and the like.
In the technical scheme provided by the invention, the purity standards of the organic solvent are analytical purity.
The invention has the beneficial effects that:
1. the invention provides a method for extracting tannic acid by utilizing dendrobium, the extracted tannic acid has excellent quality, white color, 94.7 percent of purity and 92.3 percent of extraction rate, and is mainly applied to the clinical medicine fields of protecting the wall of an artery, preventing arteriosclerosis, regulating and controlling cholesterol, inhibiting platelet coagulation, preventing thrombus, protecting heart blood vessels and the like;
2. the invention provides a novel tannin extraction method and extraction raw materials, the utilization rate and the utilization value of dendrobe are improved, tannic acid extracted from dendrobe has obvious and strong effects in the fields of food, chemical industry, cosmetics, medicine and the like, and the medical effect of the same amount of tannin is 3-7% greater than that of tannin extracted from schisandra chinensis.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the technical solutions provided by the present invention include not only the contents shown in the examples.
Example 1
The embodiment provides a method for extracting high-purity tannic acid by using dendrobium as a raw material and adopting processing technologies such as extraction, concentration, distillation, separation and purification and the like.
In the embodiment, dendrobium huoshanense, dendrobium officinale and dendrobium moniliforme are selected as extraction raw materials, the ratio of the dosage of the three raw materials is 1:1:1, and the total wet weight of the dosage of the dendrobium huoshanense is 15 kg.
In this embodiment, the mixture of acetone, methanol and water in the amount ratio of 1:1:1 is selected as the organic water solvent, the methanol is 95% of laboratory methanol, and the purity of the acetone is 99.5%.
In this embodiment, the specific method for extracting tannic acid by using dendrobe is as follows:
step one, taking 15kg of lignified dendrobium stems growing for more than three years, brushing surface dust on the stems by using a hairbrush, removing impurities, shearing the stems into 5cm long stem sections, adding an organic water solvent to completely immerse the dendrobium stem sections, and heating to 35 ℃ for soaking for 2.5 hours;
step two, adding an organic hydrosolvent which is 5 times of the stem of the dendrobium in weight portion after soaking, heating the mixture to 50 ℃ in a water bath, extracting the mixture for 10 hours at constant temperature, filtering the mixture while the mixture is hot, and taking a filtrate 1 for later use; adding 7 times of organic hydrosolvent into the filter residue, heating in water bath to 50 ℃, extracting at constant temperature for 6h, filtering while hot, taking the filtrate 2, standing the filter residue, and draining for later use;
step three, mixing the filtrate 1 and the filtrate 2, stirring clockwise for 30s, stirring anticlockwise for 1min, concentrating to 1/5 of the original volume at normal temperature and normal pressure, then heating up to distillation at normal pressure, wherein the distillation pressure is 101.5kpa, heating up to 57 ℃ from the initial temperature of the concentrated solution according to the heating rate of 5 ℃/min, keeping the temperature constant, and distilling until no distillate is discharged; then heating to 65 ℃ at the heating rate of 3 ℃/min, keeping the temperature constant, and ending the distillation when the distillate is not distilled out;
vacuum drying the distillation residue at 65 deg.C to obtain off-white powder, pulverizing, sieving with 350 mesh sieve, pulverizing the oversize part again, and sieving to obtain coarse tannin; collecting the tail gas and the distillate after cooling by the condenser pipe in the distillation process, and purifying and secondarily utilizing the distillate;
step four, adding 2 times of distilled water by weight into the crude product tannin, heating to 60 ℃ at the heating rate of 3 ℃/min, and stirring for dissolving for 30 min;
standing for 3min after dissolving uniformly, quickly freezing in a freezing chamber at 1 deg.C, refrigerating for 24 hr, taking out, standing to room temperature, filtering, and collecting filtrate;
slowly filling the filtrate into AB-8 type large-aperture adsorption resin, loading the filtrate on a column at a rate of 7ml/s, eluting by using 1 time of distilled water by weight of the filtrate after the loading on the column is finished, and then eluting by using 3 times of 95% methanol solution by weight;
the elution was started with 1ml of 1% FeCl3Collecting the eluent in a 500ml big beaker, quickly replacing the beaker with a 3L transparent glass collecting device when purple precipitate appears in the beaker, and collecting the eluent;
distilling the eluate at normal pressure with distillation pressure of 101.5kpa after adsorption and elution are finished, heating to 57 ℃ from the initial temperature of the eluate at the heating rate of 5 ℃/min, keeping the temperature constant, and distilling until no distillate is discharged; then heating to 100 ℃ at the heating rate of 8 ℃/min, keeping the temperature constant, and ending the distillation when the distillate is not distilled out;
vacuum drying the residue at 65 deg.C, pulverizing, sieving with 350 mesh sieve, pulverizing the oversize part again, and sieving to obtain the undersize part.
In this embodiment, the filter residue processing method includes:
adding 8 times of distilled water by weight into the standby filter residue, heating to 45 ℃, soaking for 12h, uniformly stirring once every 35min, filtering after soaking, adding 10 times of well water by weight into the filtrate, adding 2% of monopotassium phosphate by weight of the filtrate, uniformly stirring and dissolving, and preparing the water soluble fertilizer for spraying and irrigating the dendrobium.
In this embodiment, the filter residue is submergence once more after the stem of noble dendrobium raw materials draws, draws to add 2% weight percent potassium dihydrogen phosphate of diluent after diluting the extract, make water-soluble fertilizer spraying watering stem of noble dendrobium, effectively improve the value of utilization and the result of utilization of stem of noble dendrobium resource, increase the utilization ratio of resource, effectively prevent the emergence of wasting of resources phenomenon.
In this example, the finished tannin was a pure white powder with a purity of 94.7%, and 589.7g of tannin was extracted.
Example 2
Application of tannin in medical field is provided.
In the embodiment, 50 mice with the same growth vigor, the same weight of 100g, the same health degree, higher cholesterol content in the body and the same content are selected, the mice are marked with Arabic numerals from 1 to 50, and the mice are divided into two groups and are placed in the same living environment for feeding for 50 days.
The A group is mice 1 to 25, and the B group is mice 26 to 50.
In the feeding process, the daily food intake and the water intake of each white mouse are controlled to be 200g and 20ml respectively, the foods are foods rich in cholesterol, and 1g of tannin extracted in the example 1 is added into 200g of foods eaten by the white mice in the group A every day and is uniformly stirred; adding tannin extracted from fructus Schisandrae 1g into the food 200g of the mice in group B taken daily, and stirring.
After 50 days of feeding, the cholesterol content in 50 mice is detected.
The experimental results show that: the cholesterol content in 50 mice was reduced, and the average of the cholesterol content reduction values in 25 mice in group A was 3.5% more than the cholesterol content reduction value in 25 mice in group B.
Randomly selecting 5 mice in the group A and 5 mice in the group B, and respectively measuring the cholesterol content in vivo before and after feeding as shown in the following table:
TABLE 1
Example 3
Application of tannin in sunscreen skin care product is provided.
In the embodiment, 15 experimental control groups are selected, wherein the group A comprises 100ml of common sunscreen cream; group B comprises sunscreen cream containing tannin extracted from fructus Schisandrae 100 ml; group C included 100ml of sunscreen with the finished tannin extracted in example 1;
in the experiment, the sunscreen creams in the groups B and C are completely the same as the sunscreen creams in the group A before tannin is added, and 10g of tannin is added into each of the sunscreen creams in the groups B and C.
In this experiment, 15 mice of the same growth vigor, 100g weight and identical health degree were numbered, group a included 1 to 5 mice, group B included 6 to 10 mice, group C included 11 to 15 mice, and the same volume of mouse hair was cut at the same position on the back of each mouse.
2ml of common sunscreen cream is smeared on the hair-removed part of 5 white rats in the group A; 2ml of sunscreen cream prepared in the group B is applied to the hair-removed part of 5 white mice in the group B; 2ml of sunscreen cream prepared by the group C is applied to the hair-removed part of 5 white mice in the group C; and placing 15 mice in sunny open space, enclosing, and feeding for 5 days every morning in the same manner.
The experimental result shows that the appearance of 15 mice is blackened, the blackening process of the hair-cut parts of the mice is deeper, and the average blackening degree of the hair-cut parts of 5 mice in the group A is greater than that of the hair-cut parts of 5 mice in the group B; the average blackening degree of the hair-cut parts of 5 mice in the group B is greater than that of the hair-cut parts of 5 mice in the group C.
Through detection, tannin is added into the common sunscreen cream, the absorptivity of the sunscreen cream on ultraviolet reaches more than 98 percent, and the sunscreen cream has obvious resistance to solar dermatitis and various color spots.
And through experimental comparison, the experimental result shows that:
the absorption degree of tannin extracted from herba Dendrobii to ultraviolet ray is greater than that of tannin extracted from fructus Schisandrae chinensis.
The invention also proves that the tannin extracted from dendrobium nobile has high utilization value in the aspects of food, chemical industry and the like by virtue of white rat experiments, and the action effect of the tannin is greater than that of the common tannin in related fields, so that the detailed description is omitted.
In conclusion, the method for extracting tannin by using dendrobe and the finished product tannin extracted by the method provided by the invention have significant breakthroughs in the related technical fields.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any modifications, equivalent variations and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the present invention without departing from the technical spirit of the present invention.
Claims (1)
1. A method for extracting tannic acid by using dendrobe is characterized by comprising the following steps:
a. cleaning a large amount of dendrobium stems with surface dust by using a brush, removing impurities, shearing into stem sections with the length of 4-5 cm, adding an organic hydrosolvent to completely immerse the dendrobium stems, and heating to 35 ℃ for soaking for 2-2.5 h; the organic water solvent is a mixture of acetone, methanol and water, and the dosage ratio of the acetone to the methanol to the water is 1:1: 1; the methanol is 95% of laboratory methanol, and the purity of the acetone is 99.5%;
b. adding an organic hydrosolvent which is 5-7 times of the stem of the dendrobium stem in weight part after soaking, heating in a water bath to 45-50 ℃, extracting at constant temperature for 8-10 h, filtering while hot, and taking a filtrate 1 for later use; adding organic hydrosolvent which is 7-8 times of the weight of the filter residue into the filter residue, heating the mixture in a water bath to 45-50 ℃, extracting the mixture for 5-6 hours at a constant temperature, filtering the mixture while the mixture is hot, and taking a filtrate 2; standing the filter residue, draining for later use, adding 8 times of distilled water by weight into the filter residue for later use, heating to 45 ℃, soaking for 12-14 h, uniformly stirring once every 35min, filtering after soaking, adding 10 times of well water by weight into the filtrate, adding 2% of monopotassium phosphate by weight into the filtrate, uniformly stirring and dissolving to prepare a water soluble fertilizer for spraying and irrigating the dendrobium nobile;
c. mixing the filtrate 1 and the filtrate 2, stirring clockwise for 30s, stirring anticlockwise for 1min, concentrating at room temperature and normal pressure to 1/5 of the original volume, then heating up to distill at normal pressure, wherein the distilling pressure is 101.5kpa, heating up to 57 ℃ from the initial temperature of the concentrated solution according to the heating rate of 5 ℃/min, keeping the temperature constant, and distilling until no distillate is distilled; then heating to 65 ℃ at the heating rate of 3 ℃/min, keeping the temperature constant, and ending the distillation when no distillate is distilled out;
vacuum drying the distillation residue at 65 deg.C to obtain off-white powder, pulverizing, sieving with 350 mesh sieve, pulverizing the oversize part again, and sieving to obtain coarse tannin;
d. and (3) purifying crude tannin: adding 2-3 times of distilled water by weight into the crude tannin, heating to 60 ℃ at a heating rate of 3 ℃/min, and stirring for dissolving for 30-35 min;
standing for 3min after uniform dissolution, quickly freezing in a freezing chamber at the temperature of 1-3 ℃, refrigerating for 24-25 h, taking out, standing to room temperature, and filtering to obtain a filtrate;
slowly filling the filtrate into AB-8 type large-aperture adsorption resin, loading the filtrate on a column at a rate of 7ml/s, eluting by using 1 time of distilled water by weight of the filtrate after the loading on the column is finished, and then eluting by using 3 times of 95% methanol solution by weight;
the elution was started with 1ml of 1% FeCl3Collecting the eluent in a 500ml big beaker, quickly replacing the beaker with a 1-5L transparent glass collecting device when purple precipitate appears in the beaker, and collecting the eluent;
distilling the collected eluent under normal pressure after adsorption and elution are finished, taking residues for vacuum drying at the temperature of 65-68 ℃ after the solvent is completely distilled, crushing and sieving the residues through a 350-mesh sieve, crushing the part above the sieve again and sieving the crushed part, and taking the part below the sieve as the finished product tannin;
the normal pressure distillation method of the eluent is to control the distillation pressure to be 101.5kpa, firstly, the temperature is raised to 57 ℃ from the initial temperature of the eluent according to the temperature raising rate of 5 ℃/min, the temperature is kept constant, and the distillation is carried out until no distillate is distilled out; then heating to 100 ℃ at the heating rate of 8 ℃/min, keeping the temperature constant, and ending the distillation when no distillate is distilled out;
wherein the herba Dendrobii comprises one or more of herba Dendrobii, herba Cymbopogonis Citrari, herba Verbenae, herba Dendrobii, and herba Dendrobii.
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| Evaluation of two methods for the extraction of antioxidants from medicinal plants;Hua-Bin Li et al.;《Anal Bioanal Chem》;20070327;第388卷;第483-488页 * |
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| CN108164572A (en) | 2018-06-15 |
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