CN115381892A - Preparation method of blackberry lily extract - Google Patents
Preparation method of blackberry lily extract Download PDFInfo
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- CN115381892A CN115381892A CN202211242258.3A CN202211242258A CN115381892A CN 115381892 A CN115381892 A CN 115381892A CN 202211242258 A CN202211242258 A CN 202211242258A CN 115381892 A CN115381892 A CN 115381892A
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- 241000596154 Belamcanda Species 0.000 title claims abstract description 82
- 239000000284 extract Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 161
- 239000011347 resin Substances 0.000 claims abstract description 43
- 229920005989 resin Polymers 0.000 claims abstract description 43
- 238000005303 weighing Methods 0.000 claims abstract description 32
- 239000003480 eluent Substances 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002791 soaking Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 238000011068 loading method Methods 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 230000001376 precipitating effect Effects 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000000645 desinfectant Substances 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000007689 inspection Methods 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 230000000249 desinfective effect Effects 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims 1
- 208000006673 asthma Diseases 0.000 abstract description 6
- 206010011224 Cough Diseases 0.000 abstract description 5
- 206010062717 Increased upper airway secretion Diseases 0.000 abstract description 5
- 208000026435 phlegm Diseases 0.000 abstract description 5
- 239000003053 toxin Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000035876 healing Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P11/00—Drugs for disorders of the respiratory system
- A61P11/06—Antiasthmatics
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P11/00—Drugs for disorders of the respiratory system
- A61P11/10—Expectorants
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P11/00—Drugs for disorders of the respiratory system
- A61P11/14—Antitussive agents
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Abstract
The invention discloses a preparation method of a blackberry lily extract, which comprises the following steps: s1, weighing the dried blackberry lily and placing the blackberry lily on an operation table for preparation operation; s2, soaking the weighed blackberrylily rhizome in ethanol in a certain proportion, extracting for about 3 times, and filtering and recovering the soaked ethanol to obtain a pre-extracting solution; s3, mixing D 101 Standing the porous resin on an operation table, and loading the pre-extraction solution on the container D 101 A fully porous resin column; s4, eluting with water (1-8) times of the amount of the resin v/w, eluting with 80% -100% ethanol (8-15) times of the amount of the resin v/w to obtain ethanol eluate, and collecting with a solvent barrel; and S5, filtering the ethanol eluent. The present invention providesThe preparation method of the belamcanda chinensis extract is simple and convenient in preparation process, and the belamcanda chinensis extract has an important healing effect on heat-toxin phlegm-fire stagnation and cough and asthma, greatly improves the practicability of the preparation of the belamcanda chinensis extract, and is beneficial to practical application and operation.
Description
Technical Field
The invention belongs to the technical field of blackberry lily extracts, and particularly relates to a preparation method of a blackberry lily extract.
Background
At present, the blackberry lily extract is an extract of dried rhizome of blackberry lily of Iridaceae, mainly contains flavonoid and other components, is also named as horse tiger fan and Bidens bipinnata fan, is bitter and cold in nature, has the effects of clearing heat and removing toxicity, eliminating phlegm and relieving sore throat, and is commonly used for heat-toxin phlegm-fire stagnation, sore throat, abundant phlegm and saliva, cough and asthma.
In actual life, the pharmacological action of the blackberry lily extract is wide, and the action is mainly summarized into six points: 1. the traditional Chinese medicine composition has the effects of resisting inflammation, inhibiting the increase of the permeability of the skin capillary vessels of rats caused by acetic acid, inhibiting hyaluronidase edema of the rats and the like, reducing blood pressure, continuously reducing the blood pressure by using belamcanda chinensis alcohol extract, inhibiting common pathogenic dermatophytes, inhibiting viruses, particularly viruses and other viruses in throat diseases, enhancing salivary secretion, and quickly improving the permeability of the capillary vessels, and promoting urination.
Therefore, the blackberry lily extract plays an important role in actual life, has a better treatment effect on patients with cough, asthma and sore throat, and is particularly important, but in the prior art, the blackberry lily extract method is already formed, but in the preparation of the existing blackberry lily extract, the operation is more complicated, more errors are easy to occur, the practicability of the preparation method of the blackberry lily extract is greatly reduced, and the actual application and operation are not facilitated.
The invention content is as follows:
the present invention is directed to solving the above problems by providing a method for preparing an extract of belamcanda chinensis, which solves the problems mentioned in the background art.
In order to solve the above problems, the present invention provides a technical solution:
a preparation method of a blackberry lily extract comprises the following steps:
s1, weighing the dried blackberry lily and placing the weighed blackberry lily on an operation table for preparation operation;
s2, soaking the weighed blackberrylily rhizome in ethanol in a certain proportion, extracting for about 3 times, and filtering and recovering the soaked ethanol to obtain a pre-extracting solution;
s3, mixing D 101 Standing the porous resin on an operation table, and loading the pre-extraction solution on the container D 101 A fully porous resin column;
s4, eluting with water (1-8) times of the amount of the resin v/w, eluting with 80% -100% ethanol (8-15) times of the amount of the resin v/w to obtain ethanol eluate, and collecting with a solvent barrel;
s5, filtering the ethanol eluent, controlling the temperature and then precipitating;
s6, concentrating the precipitated substances under reduced pressure to obtain paste, and drying the paste to obtain the blackberry lily extract.
Preferably, the specific manufacturing steps of the step S1 of preparing the product placed on the operation table are as follows:
s11, before preparation, the operation table needs to be disinfected;
s12, carrying out detailed inspection on the weighing instrument, weighing the weighing instrument to check whether the instrument is normal or not, and ensuring the accuracy of the preparation data;
s13, standing the dried blackberry lily in a weighing instrument for weighing, weighing 100g, and recording.
Preferably, the specific operation steps of filtering and recovering the pre-extraction liquid in the step S2 are as follows:
s21, weighing 100g of dried blackberry lily, placing the dried blackberry lily in a container, and weighing 230g of ethanol by using a weighing instrument;
s22, diluting with an appropriate amount of water and 550g of ethanol, wherein the diluted ethanol is an 80% ethanol solution;
s23, mixing and soaking 550g of 80% ethanol and 100g of dried blackberry lily while stirring, wherein the stirring operation is carried out; stirring clockwise for about 5 minutes every 15 minutes by using a stirring rod for 1 hour, observing the ethanol and the blackberry lily in detail, recording the color and the soaking softness of the blackberry lily, standing after soaking for 1 hour, extracting after standing for 20 minutes, standing after the extraction is finished, repeating the operation for 3 times, recovering the soaked ethanol by using a filtering device, placing the recovered ethanol in an empty solvent barrel, and using the recovered ethanol as a pre-extracting solution.
Preferably, the extract in step S3 is applied to D 101 The specific operation steps of the full porous resin column are as follows:
s31, using disinfectant liquid pair D 101 Sterilizing the full-porous resin, and placing the resin on a clean operation table for standing;
s32, loading the pre-extracting solution to the step D 101 Full porous resin column, D 101 The dosage of the full porous resin is 300g;
and S33, drying the mixture under reduced pressure at 70 ℃.
Preferably, the step S4 of obtaining the ethanol eluate and collecting the ethanol eluate by using a solvent bucket comprises the following specific operation steps:
S41、D 101 the full porous resin needs to be eluted with water (1-8 times of the volume of the resin) v/w, then the water is drained and 80% -100% ethanol (8-15 times of the volume of the resin) v/w is added for elution, ethanol is discharged to obtain ethanol eluent, and the ethanol eluent is collected to 100ml for subsequent operation.
Preferably, the specific steps of filtering, concentrating and precipitating the ethanol eluate in the step S5 are as follows:
s51, slowly pouring the ethanol eluent into the filter container, and precipitating for 24 hours;
s52, placing the precipitated substances into a device with the temperature of-10 ℃ for standing, wherein the precipitated substances are coagulated at a lower temperature, so that the coagulated substances are more stable and are not easy to volatilize.
Preferably, in the step S6, the precipitated substances are concentrated under reduced pressure to obtain a paste, and the paste is dried by the following specific steps:
s61, putting the precipitated substances into a closed tank, introducing oxygen into the closed tank, mixing the precipitated substances, and decompressing the inside of the substances;
s62, extruding and concentrating the decompressed substances, wherein the extrusion strength is 500mpa, so as to obtain a treated paste;
s63, drying the paste in a collection bottle at the temperature of 30 ℃ for 6 hours to obtain the blackberry lily extract.
Preferably, the time for each soaking in ethanol in the step S2 is 100-120 minutes.
Preferably, the weight of the ethanol in the step S2 is 5-10 times of that of the blackberry lily.
The beneficial effects of the invention are: the blackberry lily extract provided by the invention has the advantages that the preparation process is simple and convenient, the blackberry lily extract has an important curing effect on heat-toxin phlegm-fire stagnation and cough and asthma, the dried blackberry lily can fully react with ethanol through the mixing and stirring effects of the dried blackberry lily, the accuracy of subsequent experiments can be ensured, the precipitated substances can be placed in a device at the temperature of-10 ℃ for standing, the substances can be rapidly condensed, and further the substances can be more stable and are not easy to volatilize, the practicability of the preparation of the blackberry lily extract is greatly improved through the operation, and the actual application and operation are facilitated.
Description of the drawings:
for ease of illustration, the invention is described in detail by the following detailed description and the accompanying drawings.
Fig. 1 is a schematic flow chart of a preparation method of a blackberry lily extract.
The specific implementation mode is as follows:
as shown in fig. 1, the present embodiment adopts the following technical means.
The embodiment is as follows:
a preparation method of a blackberry lily extract comprises the following steps:
s1, weighing the dried blackberry lily and placing the weighed blackberry lily on an operation table for preparation operation, so that the authenticity of subsequent comparison data is conveniently ensured;
s2, soaking the weighed blackberrylily rhizome in ethanol with a certain proportion, extracting for about 3 times, and filtering and recovering the soaked ethanol to obtain a pre-extracting solution, so that the accuracy of data is facilitated;
s3, mixing D 101 Standing the porous resin on an operation table, and loading the pre-extraction solution on the table D 101 The full porous resin column is convenient for obtaining experimental data;
s4, eluting with water with the amount of 8 times of the resin by volume, eluting with 80% ethanol with the amount of 8 times of the resin by volume to obtain ethanol eluent, and collecting the ethanol eluent by using a solvent barrel;
s5, filtering the ethanol eluent, controlling the temperature and then precipitating;
s6, concentrating the precipitated substances under reduced pressure to obtain paste, and drying the paste to obtain the blackberry lily extract.
The specific manufacturing steps of the step S1 of placing the operation table for preparation are as follows:
s11, before preparation, disinfecting an operation table;
s12, carrying out detailed inspection on the weighing instrument, weighing the weighing instrument to check whether the instrument is normal or not, and ensuring the accuracy of the preparation data;
s13, standing the dried blackberry lily in a weighing instrument for weighing, weighing 100g of blackberry lily and recording the weighed weight.
The specific operation steps of filtering and recovering the pre-extraction liquid in the step S2 are as follows:
s21, weighing 100g of dried blackberry lily, placing the dried blackberry lily in a container, and weighing 230g of ethanol by using a weighing instrument;
s22, diluting with an appropriate amount of water and 550g of ethanol, wherein the diluted ethanol is an 80% ethanol solution;
s23, mixing and soaking 550g of 80% ethanol and 100g of dried blackberry lily while stirring, wherein the stirring operation is carried out; stirring clockwise for about 5 minutes every 15 minutes by using a stirring rod for 1 hour, observing the ethanol and the blackberry lily in detail, recording the color and the soaking softness of the blackberry lily, standing after soaking for 1 hour, extracting after standing for 20 minutes, standing after the extraction is finished, repeating the operation for 3 times, recovering the soaked ethanol by using a filtering device, placing the recovered ethanol in an empty solvent barrel, and using the recovered ethanol as a pre-extraction solution.
Wherein, the pre-extracting solution in the step S3 is loaded on the step D 101 The specific operation steps of the full porous resin column are as follows:
s31, using a disinfectant pair D 101 Sterilizing the full-porous resin, and placing the resin on a clean operation table for standing;
s32, loading the pre-extracting solution to the step D 101 Full porous resin column, D 101 The dosage of the full porous resin is 300g;
and S33, performing reduced pressure drying operation on the mixture, wherein the temperature of the reduced pressure drying is 70 ℃.
The specific operation steps of obtaining the ethanol eluent in the step S4 and collecting the ethanol eluent by using a solvent barrel are as follows:
S41、D 101 the full porous resin needs to be eluted with water 8 times of the volume of the resin v/w, then the water is drained and 80% ethanol 8 times of the volume of the resin v/w is added for elution, ethanol is discharged to obtain ethanol eluent, and the ethanol eluent is collected to 100ml for subsequent operation.
Wherein, the specific steps of filtering, concentrating and precipitating the ethanol eluent in the step S5 are as follows:
s51, slowly pouring the ethanol eluent into the filter container, and precipitating for 24 hours;
s52, placing the precipitated substances into a device with the temperature of-10 ℃ for standing, wherein the precipitated substances have a condensation phenomenon under the condition of low temperature, so that the condensed substances are more stable and are not easy to volatilize.
Wherein, in the step S6, the substances after precipitation are decompressed and concentrated to obtain paste, and the paste is dried by the following specific steps:
s61, putting the precipitated substances into a closed tank, introducing oxygen into the closed tank, mixing the precipitated substances, and decompressing the interior of the substances;
s62, extruding and concentrating the decompressed substances, wherein the extrusion strength is 500mpa, so as to obtain a treated paste;
s63, drying the paste in a collection bottle at the temperature of 30 ℃ for 6 hours to obtain the blackberry lily extract.
Wherein, the time of each ethanol soaking in the step S2 is 120 minutes.
Wherein the weight of the ethanol in the step S2 is 5 times of that of the blackberry lily.
Comparative example 1 preparation of blackberry lily extract procedure:
firstly, weighing dried blackberrylily rhizome and placing the weighed blackberrylily rhizome on an operation table for preparation operation;
secondly, soaking the weighed blackberrylily rhizome in ethanol with a certain proportion, extracting for 2 times, and filtering and recovering the soaked ethanol to obtain a pre-extracting solution;
thirdly, D is 101 Standing the porous resin on an operation table, and loading the extractive solution on the container D 101 A fully porous resin column;
step four, eluting with water with the amount of 16 times of the resin to obtain eluent, and collecting the eluent by using a solvent barrel;
fifthly, filtering the eluent, controlling the temperature and then precipitating;
and sixthly, concentrating the precipitated substances under reduced pressure to obtain paste, and drying the paste to obtain the blackberry lily extract.
The inventive example 1 and comparative example 1 were used to perform a corresponding comparative treatment, wherein 40 patients with cough and asthma were divided into 4 groups of 10 persons each, wherein 1 group was administered 5 male students and 5 female students, all had ages within the interval of 20-24, and the average age was around 22 years old; in contrast, in comparative group 1, the boys were 5, the girls were 5, all ages were within the range of 20-24, and the average age was around 22 years, in example group 2, the boys were 6, the girls were 4, the ages were within the range of 20-24, and the average age was around 22 years, while in comparative group 2, the boys were 4, the girls were 6, the ages were within the range of 20-24, and the average age was around 22 years.
The experimental method comprises the following steps: the patients were subjected to the corresponding comparative treatment, and 50ml of the blackberry lily extract prepared in example 1 was drunk by 1 group of persons per day with 50ml of warm water at 20 ℃, 50ml of the blackberry lily extract prepared in comparative example 1 was drunk by 1 group of persons per day with 50ml of warm water at 20 ℃, 50ml of the blackberry lily extract prepared in example 1 was drunk by 2 group of persons per day with 50ml of warm water at 20 ℃, and 50ml of the blackberry lily extract prepared in comparative example 1 was drunk by 2 group of persons per day with 50ml of warm water at 20 ℃.
The judging method comprises the following steps: neutrophil and eosinophil counts were recorded and compared in the beginning and on days 5, 10, 15, 20, 30 for most patients in the four groups, with the results shown in the table below.
Neutrophils:
eosinophils:
the normal value of neutrophils is 2000-7000ml, while eosinophils belong to one of leukocytes, which is relatively small and accounts for 4% -8%, as can be seen from the above table, after taking the medicine, the contents of neutrophils and eosinophils approach to the normal value after the fifteenth day after the patients of the examples 1 and 2 take the medicine, and the content of neutrophils and eosinophils decreases slowly with the lapse of time before the fifteenth day, which indicates that the medicine effect of the extract of the present invention is better, while the contents of neutrophils and eosinophils in the patients of the comparative groups 1 and 2 decrease slowly until the thirty day after the patients of the comparative groups 1 and 2, which indicates that the contents of neutrophils and eosinophils do not enter the normal range and the asthma of some patients does not improve, so that the therapeutic effect of the blackberry lily extract prepared from the patients of the examples 1 and 2 is greater than that of the blackberry stem extract used in the comparative groups 1 and 2.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. The preparation method of the blackberry lily extract is characterized by comprising the following steps:
s1, weighing the dried blackberry lily and placing the blackberry lily on an operation table for preparation operation;
s2, soaking the weighed blackberrykiky rhizome in ethanol in a certain proportion, extracting for about 3 times, and filtering and recovering the soaked ethanol to obtain a pre-extracting solution;
s3, mixing D 101 Standing the porous resin on an operation table, and loading the extractive solution on the container D 101 A fully porous resin column;
s4, eluting with water (1-8) times of the amount of the resin v/w, eluting with 80% -100% ethanol (8-15) times of the amount of the resin v/w to obtain ethanol eluate, and collecting with a solvent bucket;
s5, filtering the ethanol eluent, controlling the temperature and then precipitating;
s6, concentrating the precipitated substances under reduced pressure to obtain paste, and drying the paste to obtain the blackberry lily extract.
2. The preparation method of the blackberry lily extract according to claim 1, wherein the specific preparation steps of the preparation method in step S1, which are placed on an operation table, are as follows:
s11, before preparation, the operation table needs to be disinfected;
s12, carrying out detailed inspection on the weighing instrument, weighing the weighing instrument to check whether the instrument is normal or not, and ensuring the accuracy of the preparation data;
s13, standing the dried blackberry lily in a weighing instrument for weighing, weighing 100g, and recording.
3. The method for preparing blackberry lily extract according to claim 1, wherein the specific operation steps of filtering and recovering the pre-extract in the step S2 are as follows:
s21, weighing 100g of dried blackberry lily, placing the dried blackberry lily in a container, and weighing 230g of ethanol by using a weighing instrument;
s22, diluting with an appropriate amount of water and 550g of ethanol, wherein the diluted ethanol is an 80% ethanol solution;
s23, mixing and soaking 550g of 80% ethanol and 100g of dried blackberry lily while stirring, wherein the stirring operation is carried out; stirring clockwise for about 5 minutes every 15 minutes by using a stirring rod for 1 hour, observing the ethanol and the blackberry lily in detail, recording the color and the soaking softness of the blackberry lily, standing after soaking for 1 hour, extracting after standing for 20 minutes, standing after the extraction is finished, repeating the operation for 3 times, recovering the soaked ethanol by using a filtering device, placing the recovered ethanol in an empty solvent barrel, and using the recovered ethanol as a pre-extracting solution.
4. The method of claim 3, wherein the extract of step S3 is applied to the treated D 101 The specific operation steps of the full porous resin column are as follows:
s31, disinfecting the full-porous resin by using a disinfectant, and placing the all-porous resin on a clean operation table for standing;
s32, loading the pre-extracting solution to the step D 101 Full porous resin column, D 101 The dosage of the full porous resin is 300g;
and S33, drying the mixture under reduced pressure at 70 ℃.
5. The method for preparing blackberry lily extract according to claim 1, wherein the ethanol eluent obtained in step S4 is collected by using a solvent bucket, and the specific operation steps are as follows:
S41、D 101 the full-porous resin needs to be eluted with water (1-8) times of the amount of the resin by volume, then the water is drained and added with 80% -100% ethanol (8-15) times of the amount of the resin by volume for elution, the ethanol is drained to obtain ethanol eluent, and the ethanol eluent which is collected to 100ml is used for subsequent operation.
6. The method for preparing blackberry lily extract according to claim 1, wherein the step S5 of filtering the ethanol eluate, concentrating and precipitating comprises the following steps:
s51, slowly pouring the ethanol eluent into the filter container, and precipitating for 24 hours;
s52, placing the precipitated substances into a device with the temperature of-10 ℃ for standing, wherein the precipitated substances are coagulated at a lower temperature, so that the coagulated substances are more stable and are not easy to volatilize.
7. The method for preparing blackberry lily extract according to claim 1, wherein the step S6 is to concentrate the precipitated substances under reduced pressure to obtain paste, and then the step of drying the paste is as follows:
s61, putting the precipitated substances into a closed tank, introducing oxygen into the closed tank, mixing the precipitated substances, and decompressing the inside of the substances;
s62, extruding and concentrating the decompressed substances, wherein the extrusion strength is 500mpa, so as to obtain a treated paste;
s63, drying the paste in a collection bottle at the temperature of 30 ℃ for 6 hours to obtain the blackberry lily extract.
8. The method for preparing blackberry lily extract according to claim 2, wherein the time for each ethanol soaking in step S2 is 100-120 minutes.
9. The method for preparing blackberry lily extract according to claim 2, wherein the weight of ethanol in step S2 is 5-10 times of that of blackberry lily.
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| 尤献民等: ""射干有效组分大孔吸附树脂分离特性的研究"", 《辽宁中医杂志》, vol. 40, no. 11, pages 2328 - 2330 * |
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