CN114558050A - Preparation method of traditional Chinese medicine stephania tetrandra extract - Google Patents
Preparation method of traditional Chinese medicine stephania tetrandra extract Download PDFInfo
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- CN114558050A CN114558050A CN202210277088.6A CN202210277088A CN114558050A CN 114558050 A CN114558050 A CN 114558050A CN 202210277088 A CN202210277088 A CN 202210277088A CN 114558050 A CN114558050 A CN 114558050A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000003814 drug Substances 0.000 title claims abstract description 17
- 241001369613 Stephania tetrandra Species 0.000 title claims description 50
- 238000011282 treatment Methods 0.000 claims abstract description 139
- 238000002386 leaching Methods 0.000 claims abstract description 86
- 238000004880 explosion Methods 0.000 claims abstract description 76
- 238000002791 soaking Methods 0.000 claims abstract description 34
- 238000000227 grinding Methods 0.000 claims abstract description 25
- 238000000605 extraction Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 41
- 238000000944 Soxhlet extraction Methods 0.000 claims description 22
- 238000000746 purification Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 14
- 238000004440 column chromatography Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 108010059892 Cellulase Proteins 0.000 claims description 10
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 10
- 108010059820 Polygalacturonase Proteins 0.000 claims description 10
- 229940106157 cellulase Drugs 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 108010093305 exopolygalacturonase Proteins 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 108010002430 hemicellulase Proteins 0.000 claims description 10
- 229940059442 hemicellulase Drugs 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims 1
- 239000004480 active ingredient Substances 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000009210 therapy by ultrasound Methods 0.000 abstract description 2
- 229940126680 traditional chinese medicines Drugs 0.000 abstract description 2
- WVTKBKWTSCPRNU-KYJUHHDHSA-N (+)-Tetrandrine Chemical compound C([C@H]1C=2C=C(C(=CC=2CCN1C)OC)O1)C(C=C2)=CC=C2OC(=C2)C(OC)=CC=C2C[C@@H]2N(C)CCC3=CC(OC)=C(OC)C1=C23 WVTKBKWTSCPRNU-KYJUHHDHSA-N 0.000 description 32
- WVTKBKWTSCPRNU-UHFFFAOYSA-N rac-Tetrandrin Natural products O1C(C(=CC=2CCN3C)OC)=CC=2C3CC(C=C2)=CC=C2OC(=C2)C(OC)=CC=C2CC2N(C)CCC3=CC(OC)=C(OC)C1=C23 WVTKBKWTSCPRNU-UHFFFAOYSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- 239000000706 filtrate Substances 0.000 description 6
- 206010042674 Swelling Diseases 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008961 swelling Effects 0.000 description 3
- 201000004624 Dermatitis Diseases 0.000 description 2
- 206010061218 Inflammation Diseases 0.000 description 2
- 208000002193 Pain Diseases 0.000 description 2
- 208000003251 Pruritus Diseases 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000003266 anti-allergic effect Effects 0.000 description 2
- 230000036737 immune function Effects 0.000 description 2
- 230000004054 inflammatory process Effects 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 230000007803 itching Effects 0.000 description 2
- 230000036407 pain Effects 0.000 description 2
- 208000024891 symptom Diseases 0.000 description 2
- 206010012442 Dermatitis contact Diseases 0.000 description 1
- 206010015150 Erythema Diseases 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 239000003470 adrenal cortex hormone Substances 0.000 description 1
- 239000013566 allergen Substances 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000000172 allergic effect Effects 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000001139 anti-pruritic effect Effects 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 208000010247 contact dermatitis Diseases 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 230000000773 effect on pain Effects 0.000 description 1
- IIQSJHUEZBTSAT-VMPREFPWSA-N fangchinoline Chemical compound C([C@H]1C=2C=C(C(=CC=2CCN1C)OC)O1)C(C=C2)=CC=C2OC(=C2)C(OC)=CC=C2C[C@@H]2N(C)CCC3=CC(OC)=C(O)C1=C23 IIQSJHUEZBTSAT-VMPREFPWSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 208000004296 neuralgia Diseases 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010898 silica gel chromatography Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
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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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/59—Menispermaceae (Moonseed family), e.g. hyperbaena or coralbead
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/395—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
- A61K31/435—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having six-membered rings with one nitrogen as the only ring hetero atom
- A61K31/47—Quinolines; Isoquinolines
- A61K31/4748—Quinolines; Isoquinolines forming part of bridged ring systems
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- 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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- 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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
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- 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
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- 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
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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Abstract
The invention discloses a preparation method of a traditional Chinese medicine radix stephaniae tetrandrae extract, belonging to the technical field of extraction of active ingredients of traditional Chinese medicines, and comprising the following steps: (1) soaking treatment; (2) carrying out continuous flash explosion treatment; (3) carrying out superfine grinding treatment; (4) primary leaching; (5) deep cooling and crushing; (6) secondary leaching: (7) and (5) purifying. The application applies the technologies of soaking, ultrasonic treatment, flash explosion treatment and the like to the preparation of the tetrandra root extract, can effectively improve the extraction rate of active ingredients and improve the bioavailability of the tetrandra root.
Description
Technical Field
The invention belongs to the technical field of extraction of active ingredients of traditional Chinese medicines, and particularly relates to a preparation method of a traditional Chinese medicine radix stephaniae tetrandrae extract.
Background
Tetrandrine has the following functions: (1) anti-allergy: it has anti-allergic effect similar to that of adrenocortical hormone, but has no influence on the immune function of body. (2) Diminishing inflammation: a broad-spectrum antiinflammatory medicine has effect in inhibiting contact dermatitis due to corticoids. (3) Analgesia: has obvious inhibition effect on pain and neuralgia caused by allergy and edema. (4) Swelling reduction: can effectively inhibit skin red swelling, itching and pain caused by allergen. (5) And (3) regulating immunity: the fundamental reason of skin allergy is that the immune system of the skin is destroyed, the barrier function of the skin is lost, the tetrandrine can restore the normal immune function of the skin, the resistance to external stimulation is enhanced, and the problem of skin allergy is fundamentally solved. (6) The tetrandrine has obvious inhibition effect on allergic symptoms such as itching pain, red swelling, inflammation and the like caused by various sensitizers, and the symptoms can be obviously relieved after 0.5 percent of tetrandrine is used for 30 minutes. The tetrandrine with 2 percent of the content has obvious immediate analgesic and antipruritic effects.
At present, active ingredients in tetrandra are researched more liquid, but the extraction of the active ingredients is often insufficient, especially the yield of tetrandrine is low, and the tetrandrine is not fully utilized.
Disclosure of Invention
The invention aims to solve the existing problems and provides a preparation method of a traditional Chinese medicine stephania tetrandra extract.
The invention is realized by the following technical scheme:
a preparation method of a traditional Chinese medicine stephania tetrandra extract comprises the following steps:
(1) soaking treatment:
immersing the dried root of tetrandra root in the treatment liquid, and then placing the treatment liquid in an ultrasonic environment for shaking treatment;
(2) continuous flash explosion treatment:
after soaking, filtering out, putting into a continuous flash explosion machine for continuous flash explosion treatment, and taking out for later use after soaking;
(3) ultramicro crushing treatment:
drying the stephania tetrandra root subjected to the continuous flash explosion treatment in the step (2) at a low temperature, and then placing the stephania tetrandra root into an ultrafine grinder for ultrafine grinding treatment to obtain stephania tetrandra root powder for later use;
(4) primary leaching:
placing the tetrandra powder obtained in the step (3) into a Soxhlet extraction device for primary extraction to obtain primary extract and filter residue for later use;
(5) cryogenic crushing:
placing the filter residue obtained in the step (4) into a pre-cooled cryogenic grinder, freezing for 10-20 s, and immediately grinding to obtain filter residue powder for later use;
(6) secondary leaching:
placing the filter residue powder obtained in the step (5) into a Soxhlet extraction device for secondary leaching to obtain secondary leaching liquor for later use:
(7) and (3) purification:
and (4) concentrating the primary leaching solution obtained in the step (4) and the secondary leaching solution obtained in the step (6) into leaching paste, dissolving, mixing samples, and performing column chromatography purification.
Further, the treating fluid in the step (1) comprises the following components in percentage by weight: 0.7-0.9% of cellulase, 1-2% of hemicellulase, 0.6-0.8% of pectinase, 2-3% of ethylenediamine and the balance of water.
Further, the shaking speed in the shaking treatment in the step (1) is 100-120 rpm, and the time of the shaking treatment is 1-2 h.
Further, the frequency of the ultrasonic wave in the step (1) is 30-50 kHz.
Further, the rotating speed of the flash explosion machine during the flash explosion treatment in the step (2) is 700-800 rpm, and the number of flash explosion treatments is 20-30.
Further, the rotation speed of the pulverizer during the superfine grinding treatment in the step (3) is 20000-30000 rpm, and the grinding treatment time is 3-5 min.
Further, the time of the primary leaching in the step (4) is 3-4 hours.
Further, the precooling temperature in the step (5) is-80 to-60 ℃.
Further, the rotating speed of the pulverizer in the pulverizing treatment in the step (5) is 1000-2000 rpm, and the pulverizing treatment time is 6-9 min.
Further, the time of the secondary leaching in the step (6) is 1-2 hours.
Compared with the prior art, the invention has the following advantages:
1. the method is improved to a great extent on the basis of the existing extraction means, and the yield of the active ingredients is effectively improved. Firstly, dry roots of tetrandra root are immersed into a treatment solution, the soaking treatment is carried out under the auxiliary action of shaking and ultrasonic waves, the degree of polymerization of fibers in the tetrandra root is effectively reduced, the thread hole rate of cells is improved, then the permeability and the thread hole rate of the cells are further improved under the action of continuous flash explosion, the obtained powder has better solubility and dispersibility through ultramicro crushing treatment, repeated reflux extraction is carried out by utilizing a Soxhlet extraction device, the filter residue is rapidly frozen under the ultralow temperature condition and then is subjected to deep cooling crushing treatment, due to the rapid freezing, an extremely large internal and external temperature difference can be generated in an extremely short time, then crushing is carried out, the crushing is more thorough, the crushed powder is subjected to secondary extraction, effective components are fully dissolved out, and the yield of the tetrandrine is obviously improved.
2. The application applies the technologies of soaking, ultrasonic treatment, flash explosion treatment and the like to the preparation of the tetrandra root extract, can effectively improve the extraction rate of active ingredients and improve the bioavailability of the tetrandra root.
Detailed Description
Example 1:
a preparation method of a traditional Chinese medicine stephania tetrandra extract comprises the following steps:
(1) soaking treatment:
immersing dried roots of tetrandra root into a treatment solution, then placing the treatment solution in an ultrasonic environment for shaking treatment at the speed of 100rpm for 1h, wherein the frequency of ultrasonic waves is 30kHz, and the treatment solution comprises the following components in percentage by weight: 0.7% of cellulase, 1% of hemicellulase, 0.6% of pectinase, 2% of ethylenediamine and the balance of water;
(2) continuous flash explosion treatment:
after soaking, filtering out the filtrate, putting the filtrate into a continuous flash explosion machine for continuous flash explosion treatment, wherein the rotating speed of the flash explosion machine is 700rpm, the number of flash explosion treatment is 20, and taking out the filtrate for later use after the flash explosion treatment is finished;
(3) ultramicro crushing treatment:
drying the stephania tetrandra roots subjected to the continuous flash explosion treatment in the step (2) at a low temperature, and then placing the stephania tetrandra roots into an ultrafine grinder for ultrafine grinding treatment, wherein the rotation speed of the grinder is 20000rpm, and grinding for 3min to obtain stephania tetrandra powder for later use;
(4) primary leaching:
placing the tetrandra powder obtained in the step (3) into a Soxhlet extraction device for primary extraction, and extracting for 3 hours to obtain primary extract and filter residue for later use;
(5) cryogenic crushing:
placing the filter residue obtained in the step (4) in a precooling type cryogenic grinder, wherein the precooling temperature is-80 ℃, the filter residue is frozen for 10s and then immediately ground, the rotating speed of the grinder is 1000rpm, and the filter residue powder is obtained for standby after grinding for 6 min;
(6) secondary leaching:
placing the filter residue powder obtained in the step (5) into a Soxhlet extraction device for secondary leaching, and leaching for 1h to obtain a secondary leaching solution for later use:
(7) and (3) purification:
and (4) concentrating the primary leaching solution obtained in the step (4) and the secondary leaching solution obtained in the step (6) into leaching paste, dissolving, mixing samples, and performing column chromatography purification.
Example 2:
a preparation method of a traditional Chinese medicine stephania tetrandra extract comprises the following steps:
(1) soaking treatment:
immersing dried roots of tetrandra root into a treatment solution, then placing the treatment solution in an ultrasonic environment for shaking treatment at the speed of 110rpm for 1.5h, wherein the frequency of ultrasonic waves is 40kHz, and the treatment solution comprises the following components in percentage by weight: 0.8% of cellulase, 1.5% of hemicellulase, 0.7% of pectinase, 2.5% of ethylenediamine and the balance of water;
(2) continuous flash explosion treatment:
filtering out after soaking, placing in a continuous flash explosion machine for continuous flash explosion treatment, wherein the rotating speed of the flash explosion machine is 750rpm, the number of flash explosion treatment is 25, and taking out for later use after soaking;
(3) ultramicro crushing treatment:
drying the stephania tetrandra roots subjected to the continuous flash explosion treatment in the step (2) at a low temperature, and then placing the stephania tetrandra roots into an ultrafine grinder for ultrafine grinding treatment, wherein the rotation speed of the grinder is 25000rpm, and the stephania tetrandra roots are ground for 4min to obtain stephania tetrandra powder for later use;
(4) primary leaching:
placing the tetrandra powder obtained in the step (3) into a Soxhlet extraction device for primary extraction, and extracting for 3.5 hours to obtain primary extract and filter residue for later use;
(5) cryogenic crushing:
placing the filter residue obtained in the step (4) in a precooling type cryogenic grinder, wherein the precooling temperature is-70 ℃, the filter residue is frozen for 15s and then immediately ground, the rotating speed of the grinder is 1500rpm, and the filter residue powder is obtained for standby after grinding for 7.5 min;
(6) secondary leaching:
placing the filter residue powder obtained in the step (5) into a Soxhlet extraction device for secondary leaching, and leaching for 1.5h to obtain secondary leaching liquor for later use:
(7) and (3) purification:
and (4) concentrating the primary leaching solution obtained in the step (4) and the secondary leaching solution obtained in the step (6) into leaching paste, dissolving, mixing samples, and performing column chromatography purification.
Example 3:
a preparation method of a traditional Chinese medicine radix stephaniae tetrandrae extract comprises the following steps:
(1) soaking treatment:
immersing dried roots of tetrandra root into a treatment solution, then placing the treatment solution in an ultrasonic environment for shaking treatment at the speed of 120rpm for 2h, wherein the frequency of ultrasonic waves is 50kHz, and the treatment solution comprises the following components in percentage by weight: 0.9% of cellulase, 2% of hemicellulase, 0.8% of pectinase, 3% of ethylenediamine and the balance of water;
(2) continuous flash explosion treatment:
after soaking, filtering out the filtrate, putting the filtrate into a continuous flash explosion machine for continuous flash explosion treatment, wherein the rotating speed of the flash explosion machine is 800rpm, the number of flash explosion treatment is 30, and taking out the filtrate for later use after the flash explosion treatment is finished;
(3) ultramicro crushing treatment:
drying the stephania tetrandra roots subjected to the continuous flash explosion treatment in the step (2) at a low temperature, and then placing the stephania tetrandra roots into an ultrafine grinder for ultrafine grinding treatment, wherein the rotating speed of the grinder is 30000rpm, and grinding for 5min to obtain stephania tetrandra powder for later use;
(4) primary leaching:
placing the tetrandra powder obtained in the step (3) into a Soxhlet extraction device for primary extraction, and extracting for 4 hours to obtain primary extract and filter residue for later use;
(5) cryogenic crushing:
placing the filter residue obtained in the step (4) in a precooling type cryogenic grinder, wherein the precooling temperature is-60 ℃, the filter residue is frozen for 20s and then immediately ground, the rotating speed of the grinder is 2000rpm, and the filter residue powder is obtained for standby after grinding for 9 min;
(6) secondary leaching:
placing the filter residue powder obtained in the step (5) in a Soxhlet extraction device for secondary leaching for 2 hours to obtain secondary leaching liquor for later use:
(7) and (3) purification:
and (4) concentrating the primary leaching solution obtained in the step (4) and the secondary leaching solution obtained in the step (6) into leaching paste, dissolving, mixing samples, and performing column chromatography purification.
For further explanation of the present invention, reference will now be made to the following specific examples.
Comparative example 1:
a preparation method of a traditional Chinese medicine radix stephaniae tetrandrae extract comprises the following steps:
(1) soaking treatment:
soaking the dried root of tetrandra root in a treatment solution for 1.5h, wherein the treatment solution comprises the following components in percentage by weight: 0.8% of cellulase, 1.5% of hemicellulase, 0.7% of pectinase, 2.5% of ethylenediamine and the balance of water;
(2) continuous flash explosion treatment:
filtering out after soaking, placing in a continuous flash explosion machine for continuous flash explosion treatment, wherein the rotating speed of the flash explosion machine is 750rpm, the number of flash explosion treatment is 25, and taking out for later use after soaking;
(3) ultramicro crushing treatment:
drying the stephania tetrandra roots subjected to the continuous flash explosion treatment in the step (2) at a low temperature, and then placing the stephania tetrandra roots into an ultrafine grinder for ultrafine grinding treatment, wherein the rotation speed of the grinder is 25000rpm, and the stephania tetrandra roots are ground for 4min to obtain stephania tetrandra powder for later use;
(4) primary leaching:
placing the tetrandra powder obtained in the step (3) into a Soxhlet extraction device for primary extraction, and extracting for 3.5 hours to obtain primary extract and filter residue for later use;
(5) cryogenic crushing:
placing the filter residue obtained in the step (4) in a precooling type cryogenic grinder, wherein the precooling temperature is-70 ℃, the filter residue is frozen for 15s and then immediately ground, the rotating speed of the grinder is 1500rpm, and the filter residue powder is obtained for standby after grinding for 7.5 min;
(6) secondary leaching:
placing the filter residue powder obtained in the step (5) into a Soxhlet extraction device for secondary leaching for 1.5h to obtain secondary leaching liquor for later use:
(7) and (3) purification:
and (4) concentrating the primary leaching solution obtained in the step (4) and the secondary leaching solution obtained in the step (6) into leaching paste, dissolving, mixing samples, and performing column chromatography purification.
Comparative example 2:
a preparation method of a traditional Chinese medicine radix stephaniae tetrandrae extract comprises the following steps:
(1) continuous flash explosion treatment:
putting the dried root of tetrandra root into a continuous flash explosion machine for continuous flash explosion treatment, wherein the rotating speed of the flash explosion machine is 750rpm, the number of flash explosion treatment is 25, and taking out the dried root for later use after the flash explosion treatment is finished;
(2) ultramicro crushing treatment:
drying the stephania tetrandra roots subjected to the continuous flash explosion treatment in the step (2) at a low temperature, and then placing the stephania tetrandra roots into an ultrafine grinder for ultrafine grinding treatment, wherein the rotation speed of the grinder is 25000rpm, and the stephania tetrandra roots are ground for 4min to obtain stephania tetrandra powder for later use;
(3) primary leaching:
placing the tetrandra powder obtained in the step (2) into a Soxhlet extraction device for primary extraction, and extracting for 3.5 hours to obtain primary extract and filter residue for later use;
(4) cryogenic crushing:
placing the filter residue obtained in the step (3) in a precooling cryogenic grinder, wherein the precooling temperature is-70 ℃, the filter residue is frozen for 15s and then immediately ground, the rotation speed of the grinder is 1500rpm, and the filter residue powder is obtained for standby after grinding for 7.5 min;
(5) secondary leaching:
placing the filter residue powder obtained in the step (4) into a Soxhlet extraction device for secondary leaching, and leaching for 1.5h to obtain secondary leaching liquor for later use:
(6) and (3) purification:
and (4) concentrating the primary leaching solution obtained in the step (3) and the secondary leaching solution obtained in the step (5) into leaching paste, dissolving, mixing samples, and performing column chromatography purification.
Comparative example 3:
a preparation method of a traditional Chinese medicine stephania tetrandra extract comprises the following steps:
(1) soaking treatment:
immersing dried roots of tetrandra root into a treatment solution, then placing the treatment solution in an ultrasonic environment for shaking treatment at the speed of 110rpm for 1.5h, wherein the frequency of ultrasonic waves is 40kHz, and the treatment solution comprises the following components in percentage by weight: 0.8% of cellulase, 1.5% of hemicellulase, 0.7% of pectinase, 2.5% of ethylenediamine and the balance of water;
(2) continuous flash explosion treatment:
filtering out after soaking, placing in a continuous flash explosion machine for continuous flash explosion treatment, wherein the rotating speed of the flash explosion machine is 750rpm, the number of flash explosion treatment is 25, and taking out for later use after soaking;
(3) primary leaching:
placing the tetrandra root subjected to flash explosion treatment in the step (2) into a Soxhlet extraction device for primary extraction, and extracting for 3.5 hours to obtain primary extract and filter residue for later use;
(4) cryogenic crushing:
placing the filter residue obtained in the step (3) in a precooling type cryogenic grinder, wherein the precooling temperature is-70 ℃, the filter residue is frozen for 15s and then immediately ground, the rotating speed of the grinder is 1500rpm, and the filter residue powder is obtained for standby after grinding for 7.5 min;
(5) secondary leaching:
placing the filter residue powder obtained in the step (4) into a Soxhlet extraction device for secondary leaching, and leaching for 1.5h to obtain secondary leaching liquor for later use:
(6) and (3) purification:
and (4) concentrating the primary leaching solution obtained in the step (3) and the secondary leaching solution obtained in the step (5) into leaching paste, dissolving, mixing samples, and performing column chromatography purification.
Comparative example 4:
a preparation method of a traditional Chinese medicine radix stephaniae tetrandrae extract comprises the following steps:
(1) soaking treatment:
immersing the dried roots of the tetrandra root into the treatment liquid, then placing the treatment liquid in an ultrasonic environment for shaking treatment, wherein the shaking speed is 110rpm, the shaking treatment time is 1.5h, the frequency of ultrasonic waves is 40kHz, and the treatment liquid comprises the following components in percentage by weight: 0.8% of cellulase, 1.5% of hemicellulase, 0.7% of pectinase, 2.5% of ethylenediamine and the balance of water;
(2) continuous flash explosion treatment:
filtering out after soaking, placing in a continuous flash explosion machine for continuous flash explosion treatment, wherein the rotating speed of the flash explosion machine is 750rpm, the number of flash explosion treatment is 25, and taking out for later use after soaking;
(3) ultramicro crushing treatment:
drying the stephania tetrandra roots subjected to the continuous flash explosion treatment in the step (2) at a low temperature, and then placing the stephania tetrandra roots into an ultrafine grinder for ultrafine grinding treatment, wherein the rotation speed of the grinder is 25000rpm, and the stephania tetrandra roots are ground for 4min to obtain stephania tetrandra powder for later use;
(4) primary leaching:
placing the tetrandra powder obtained in the step (3) into a Soxhlet extraction device for primary extraction, and extracting for 3.5 hours to obtain primary extract for later use;
(5) and (3) purification:
and (4) concentrating the primary leaching liquor obtained in the step (4) to obtain leaching paste, dissolving and mixing the leaching paste, and then performing column chromatography purification.
Comparative example 5:
a preparation method of a traditional Chinese medicine radix stephaniae tetrandrae extract comprises the following steps:
(1) soaking treatment:
immersing dried roots of tetrandra root into a treatment solution, then placing the treatment solution in an ultrasonic environment for shaking treatment at the speed of 110rpm for 1.5h, wherein the frequency of ultrasonic waves is 40kHz, and the treatment solution comprises the following components in percentage by weight: 0.8% of cellulase, 1.5% of hemicellulase, 0.7% of pectinase, 2.5% of ethylenediamine and the balance of water;
(2) continuous flash explosion treatment:
filtering out after soaking, placing in a continuous flash explosion machine for continuous flash explosion treatment, wherein the rotating speed of the flash explosion machine is 750rpm, the number of flash explosion treatment is 25, and taking out for later use after soaking;
(3) ultra-fine crushing treatment:
drying the stephania tetrandra roots subjected to the continuous flash explosion treatment in the step (2) at a low temperature, and then placing the stephania tetrandra roots into an ultrafine grinder for ultrafine grinding treatment, wherein the rotation speed of the grinder is 25000rpm, and the stephania tetrandra roots are ground for 4min to obtain stephania tetrandra powder for later use;
(4) primary leaching:
placing the tetrandra powder obtained in the step (3) into a Soxhlet extraction device for primary extraction, and extracting for 3.5 hours to obtain primary extract and filter residue for later use;
(5) cryogenic crushing:
putting the filter residue obtained in the step (4) into a cryogenic grinder for grinding treatment, wherein the rotating speed of the grinder is 1500rpm, and grinding treatment is carried out for 7.5min to obtain filter residue powder for later use;
(6) secondary leaching:
placing the filter residue powder obtained in the step (5) into a Soxhlet extraction device for secondary leaching, and leaching for 1.5h to obtain secondary leaching liquor for later use:
(7) and (3) purification:
and (4) concentrating the primary leaching solution obtained in the step (4) and the secondary leaching solution obtained in the step (6) into leaching paste, dissolving, mixing samples, and performing column chromatography purification.
Comparative example 6:
a preparation method of a traditional Chinese medicine radix stephaniae tetrandrae extract comprises the following steps:
(1) soaking treatment:
immersing dried roots of tetrandra root into a treatment solution, then placing the treatment solution in an ultrasonic environment for shaking treatment at the speed of 110rpm for 1.5h, wherein the frequency of ultrasonic waves is 40kHz, and the treatment solution comprises the following components in percentage by weight: 0.8% of cellulase, 1.5% of hemicellulase, 0.7% of pectinase, 2.5% of ethylenediamine and the balance of water;
(2) continuous flash explosion treatment:
filtering out after soaking, placing in a continuous flash explosion machine for continuous flash explosion treatment, wherein the rotating speed of the flash explosion machine is 750rpm, the number of flash explosion treatment is 25, and taking out for later use after soaking;
(3) ultramicro crushing treatment:
drying the stephania tetrandra roots subjected to the continuous flash explosion treatment in the step (2) at a low temperature, and then placing the stephania tetrandra roots into an ultrafine grinder for ultrafine grinding treatment, wherein the rotation speed of the grinder is 25000rpm, and the stephania tetrandra roots are ground for 4min to obtain stephania tetrandra powder for later use;
(4) primary leaching:
placing the tetrandra powder obtained in the step (3) into a Soxhlet extraction device for primary extraction, and extracting for 3.5 hours to obtain primary extract and filter residue for later use;
(5) secondary leaching:
placing the filter residue powder obtained in the step (4) into a Soxhlet extraction device for secondary leaching, and leaching for 1.5h to obtain secondary leaching liquor for later use:
(6) and (3) purification:
and (4) concentrating the primary leaching solution obtained in the step (4) and the secondary leaching solution obtained in the step (5) into leaching paste, dissolving, mixing samples, and performing column chromatography purification.
Control group
The application numbers are: CN201710034052.4 discloses a method for separating and preparing tetrandrine A and tetrandrine B by ion exchange and silica gel column chromatography.
In order to compare the technical effects of the application, the tetrandrine is prepared by the methods of the example 2, the comparative examples 1-6 and the control group respectively, and then the yield of the tetrandrine is determined by a liquid chromatography method.
The specific experimental comparative data are shown in the following table 1:
table 1 the tetrandrine yield results of each group of methods (n ═ 3)
| Tetrandrine yield (g/100g) | |
| Example 2 | 1.0512 |
| Comparative example 1 | 0.8622 |
| Comparative example 2 | 0.7965 |
| Comparative example 3 | 0.8326 |
| Comparative example 4 | 0.7326 |
| Comparative example 5 | 0.8136 |
| Comparative example 6 | 0.8403 |
| Control group | 0.7592 |
As can be seen from table 1 above, by adopting the above technical scheme, the application applies the technologies of soaking, ultrasonic wave, flash explosion treatment and the like to the preparation of the tetrandrine extract, which significantly improves the yield of tetrandrine and improves the bioavailability of tetrandrine.
Claims (10)
1. A preparation method of a traditional Chinese medicine radix stephaniae tetrandrae extract is characterized by comprising the following steps:
(1) soaking treatment:
immersing the dried root of tetrandra root in the treatment liquid, and then placing the treatment liquid in an ultrasonic environment for shaking treatment;
(2) continuous flash explosion treatment:
after soaking, filtering out, putting into a continuous flash explosion machine for continuous flash explosion treatment, and taking out for later use after soaking;
(3) ultramicro crushing treatment:
drying the stephania tetrandra roots subjected to the continuous flash explosion treatment in the step (2) at a low temperature, and then placing the stephania tetrandra roots in an ultrafine grinder for ultrafine grinding treatment to obtain stephania tetrandra powder for later use;
(4) primary leaching:
placing the tetrandra powder obtained in the step (3) into a Soxhlet extraction device for primary extraction to obtain primary extract and filter residue for later use;
(5) cryogenic crushing:
placing the filter residue obtained in the step (4) in a precooling cryogenic grinder, freezing for 10-20 s, and immediately grinding to obtain filter residue powder for later use;
(6) secondary leaching:
placing the filter residue powder obtained in the step (5) into a Soxhlet extraction device for secondary leaching to obtain secondary leaching liquor for later use:
(7) and (3) purification:
and (4) concentrating the primary leaching solution obtained in the step (4) and the secondary leaching solution obtained in the step (6) into leaching paste, dissolving, mixing samples, and performing column chromatography purification.
2. The method for preparing the extract of stephania tetrandra as claimed in claim 1, wherein the treating solution in step (1) comprises the following components in percentage by weight: 0.7-0.9% of cellulase, 1-2% of hemicellulase, 0.6-0.8% of pectinase, 2-3% of ethylenediamine and the balance of water.
3. The method for preparing the extract of Stephania tetrandra as claimed in claim 1, wherein the shaking speed in the shaking treatment in step (1) is 100-120 rpm, and the shaking treatment time is 1-2 h.
4. The method for preparing the extract of stephania tetrandra as claimed in claim 1, wherein the frequency of the ultrasonic wave in step (1) is 30-50 kHz.
5. The method for preparing a Chinese medicinal composition of radix Stephaniae Japonicae extract according to claim 1, wherein the rotation speed of the flash explosion machine in the flash explosion treatment of step (2) is 700-800 rpm, and the number of flash explosion treatments is 20-30 times.
6. The method for preparing the extract of stephania tetrandra as claimed in claim 1, wherein the rotation speed of the pulverizer during the micronization treatment in step (3) is 20000-30000 rpm, and the pulverization treatment time is 3-5 min.
7. The method for preparing a Chinese medicinal tetrandra root extract according to claim 1, wherein the time for the first leaching in the step (4) is 3-4 hours.
8. The method for preparing an extract of stephania tetrandra as claimed in claim 1, wherein the pre-cooling temperature in step (5) is-80 to-60 ℃.
9. The method for preparing the extract of stephania tetrandra as claimed in claim 1, wherein the rotation speed of the pulverizer is 1000-2000 rpm and the pulverizing time is 6-9 min during the pulverizing treatment in step (5).
10. The method for preparing the extract of stephania tetrandra as claimed in claim 1, wherein the time of the second leaching in step (6) is 1-2 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115120592A (en) * | 2022-06-28 | 2022-09-30 | 傅绍义 | Composition for relieving skin pruritus and allergy, clinical test method and application |
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| CN104193754A (en) * | 2014-09-04 | 2014-12-10 | 南京标科生物科技有限公司 | New method for extracting tetrandrine from radix stephaniae tetrandrae |
| CN105541857A (en) * | 2016-01-18 | 2016-05-04 | 北京七巧时代科技有限公司 | Tetrandrine extract as well as preparation method and application thereof |
| CN108218885A (en) * | 2018-01-25 | 2018-06-29 | 安徽诚亚生物科技有限公司 | A kind of extracting method of the tetrandrine of improvement |
| CN110680802A (en) * | 2019-11-11 | 2020-01-14 | 江西银涛药业有限公司 | Tetrandrine injection and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193754A (en) * | 2014-09-04 | 2014-12-10 | 南京标科生物科技有限公司 | New method for extracting tetrandrine from radix stephaniae tetrandrae |
| CN105541857A (en) * | 2016-01-18 | 2016-05-04 | 北京七巧时代科技有限公司 | Tetrandrine extract as well as preparation method and application thereof |
| CN108218885A (en) * | 2018-01-25 | 2018-06-29 | 安徽诚亚生物科技有限公司 | A kind of extracting method of the tetrandrine of improvement |
| CN110680802A (en) * | 2019-11-11 | 2020-01-14 | 江西银涛药业有限公司 | Tetrandrine injection and preparation method thereof |
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| CN115120592A (en) * | 2022-06-28 | 2022-09-30 | 傅绍义 | Composition for relieving skin pruritus and allergy, clinical test method and application |
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