CN114129522A - Cynanchum paniculatum formula granules and preparation method thereof - Google Patents

Cynanchum paniculatum formula granules and preparation method thereof Download PDF

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Publication number
CN114129522A
CN114129522A CN202111609313.3A CN202111609313A CN114129522A CN 114129522 A CN114129522 A CN 114129522A CN 202111609313 A CN202111609313 A CN 202111609313A CN 114129522 A CN114129522 A CN 114129522A
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paniculate swallowwort
decoction pieces
swallowwort root
cynanchum paniculatum
paeonol
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魏文君
吴美兰
孙立恩
陈剑
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ZHEJIANG JINGYUETANG PHARMACEUTICAL CO Ltd
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1682Processes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/27Asclepiadaceae (Milkweed family), e.g. hoya
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1629Organic macromolecular compounds
    • A61K9/1652Polysaccharides, e.g. alginate, cellulose derivatives; Cyclodextrin
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04Antibacterial agents
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    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P37/00Drugs for immunological or allergic disorders
    • A61P37/02Immunomodulators
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00Drugs for disorders of the cardiovascular system
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K31/12Ketones

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Abstract

The invention discloses a paniculate swallowwort root formula particle and a preparation method thereof, relates to the technical field of traditional Chinese medicine formula particle preparation, and aims to solve the problem of great loss of paeonol during extraction of the existing paniculate swallowwort root, and the technical scheme is characterized by comprising the following steps: (1) pre-treating; (2) extracting; (3) concentrating; (4) drying; (5) totally mixing; (6) and (5) granulating. According to the invention, the cynanchum paniculatum decoction pieces and the beta-cyclodextrin are soaked together, so that the defects of poor water solubility and easiness in volatilization of paeonol can be overcome, the stability and biological effect of the paeonol are improved, the loss of the paeonol can be effectively reduced, and the transfer rate is improved.

Description

Cynanchum paniculatum formula granules and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of traditional Chinese medicine formula granules, and particularly relates to a paniculate swallowwort root formula granule and a preparation method thereof.
Background
The radix Cynanchi Paniculati is dry root and rhizome of Cynanchum paniculatum Paniculatum Panicum (Bge.) paniculatum of Asclepiadaceae. Collected in autumn, removed impurities, dried in the shade, and has effects of dispelling pathogenic wind, eliminating dampness, relieving pain and relieving itching. The paniculate swallowwort root is a perennial herb of the genus Anemone of the family Asclepiadaceae, also called ghost, Sanbai root, Yaowang, Japanese peristrophe herb, Linchaihu herb, etc., and is a common traditional Chinese medicine and folk herbal medicine, which appears for the first time in Shennong herbal medicine. The Chinese medicinal composition is distributed in most provinces and markets of Liaoning, Hebei, Shaanxi, southwest, China, east China, south China and the like, is a common Chinese medicament income pharmacopoeia of China, and has great medicinal value. The traditional Chinese medicine composition is mainly used for treating skin diseases such as rheumatic pain, eczema, stubborn dermatitis, urticaria and the like in clinic, and can also be used for treating venomous snake bite. The current research shows that the cynanchum paniculatum extract is rich in compounds such as saturated hydrocarbons, volatile oil, acetophenone, pentacyclic triterpenes, C21 steroids, alkaloids, polysaccharides, sterols and the like, and has the effects of resisting bacteria and viruses, protecting cardiovascular system, regulating immunity, resisting tumors and the like.
The traditional Chinese medicine formula granule is prepared by carrying out water extraction, concentration, drying and granulation on single traditional Chinese medicine decoction pieces, is a granule which is taken by a patient after being mixed with water in a traditional Chinese medicine clinical formula, and is a novel formula medicine with uniform specification, uniform dosage and uniform quality standard.
Paeonol, also called paeonol, is an active ingredient extracted from dry root or whole plant of Cynanchum paniculatum of Asclepiadaceae and root bark of Paeonia suffruticosa and Paeonia lactiflora of Ranunculaceae. The research shows that the paeonol has certain curative effects of sedation, pain relief, antianaphylaxis, anti-infection and the like. In clinic, paeonol is compounded by a plurality of traditional Chinese medicines and has obvious effects on treating eczema, rheumatism, toothache, dermatitis and the like.
The paeonol as the characteristic component of the paniculate swallowwort root has low solubility in water and can volatilize along with water vapor, so that an extraction mode for avoiding loss of the paeonol is provided, and the problem to be solved by the technical personnel in the field is urgently needed.
Disclosure of Invention
The invention aims to solve the problems and provide a paniculate swallowwort root formula particle and a preparation method thereof, so as to overcome the defects of poor water solubility and easy volatilization of paeonol and improve the stability and biological efficacy of the paeonol.
The technical purpose of the invention is realized by the following technical scheme: a method for preparing paniculate swallowwort root formula granules comprises the following steps: (1) pretreatment: processing the cynanchum paniculatum medicinal material to obtain cynanchum paniculatum decoction pieces; (2) extraction: putting the cynanchum paniculatum decoction pieces into an extraction tank, adding a proper amount of beta-cyclodextrin, adding water which is 8-10 times of the material dosage of the cynanchum paniculatum decoction pieces for soaking, starting hot steam for heating, soaking at 70-85 ℃ for 70-90 minutes, filtering decoction liquid through a 300-mesh filter screen to obtain filtrate, adding water which is 6-8 times of the material dosage of the cynanchum paniculatum decoction pieces for soaking at 80 ℃ for 55-65 minutes, filtering the decoction liquid through a 300-mesh filter screen to obtain filtrate, and combining the two filtrates to obtain an extracting solution; (3) concentration: concentrating the product obtained in the extraction step at 50-80 deg.C under reduced pressure to relative density of 1.05-1.15 to obtain extract; (4) and (3) drying: weighing a proper amount of maltodextrin, adding water to dissolve the maltodextrin, mixing the solution with the extract, and then performing spray drying, wherein the air inlet temperature is controlled to be 170 ℃ and 190 ℃, and the air outlet temperature is controlled to be 70-95 ℃ to obtain extract powder; (5) total mixing: weighing appropriate amount of maltodextrin, and mixing with the extract powder to obtain total mixed powder; (6) and (3) granulating: and taking the total mixed powder, and performing dry granulation to obtain the formula granules.
The invention is further configured to: the mass ratio of the paniculate swallowwort root decoction pieces to the beta-cyclodextrin in the extraction step is 15: 1-20: 1.
through adopting above-mentioned technical scheme, through controlling its mass ratio, can enough better more draw out the paeonol composition in the sliced Cynanchum paniculatum, also can reduce unnecessary extravagant moreover.
The invention is further configured to: the method comprises the following steps of extracting by using a straight-tube extraction tank, concentrating by using a single-effect external circulation concentrator, drying by using a spray dryer, mixing by using a multidirectional motion mixer, and granulating by using a dry granulator.
By adopting the technical scheme and adopting the dry granulation process, the addition amount of auxiliary materials can be reduced, the medicinal ingredients can be prevented from contacting with solvents such as ethanol and the like, the risk of damaging the paeonol is further reduced, the stability of the paeonol in the prepared formula granules is high, and the finished product quality of the formula granules is improved.
The invention is further configured to: in the extraction step, the cynanchum paniculatum decoction pieces and the beta-cyclodextrin are soaked together.
By adopting the technical scheme, the cynanchum paniculatum decoction pieces and the beta-cyclodextrin are soaked together, so that the defects of poor water solubility and easiness in volatilization of paeonol can be overcome, the stability and the biological effect of the paeonol are improved, the loss of the paeonol can be effectively reduced, and the transfer rate is improved.
The invention is further configured to: the pretreatment step is that the paniculate swallowwort root medicinal material is removed with impurities such as residual stems and the like, is washed with water, is placed on a medicine cutting machine and is cut into short sections of 5-10mm, the paniculate swallowwort root decoction pieces are uniformly spread in an oven, the drying temperature is set to be not more than 60 ℃, is dried in the shade, and is sieved by a sieve with the diameter of a sieve hole of 1 mm.
A radix Cynanchi Paniculati granule is prepared by the preparation method of radix Cynanchi Paniculati granule.
In conclusion, the invention has the following beneficial effects:
according to the invention, the cynanchum paniculatum decoction pieces and the beta-cyclodextrin are soaked together, so that the defects of poor water solubility and easiness in volatilization of paeonol can be overcome, the stability and biological effect of the paeonol are improved, the loss of the paeonol can be effectively reduced, and the transfer rate is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a method for preparing paniculate swallowwort root formula granules comprises the following steps:
pretreatment: removing impurities such as residual stems from the cynanchum paniculatum medicinal material, washing with water, placing on a medicine cutting machine, cutting into short sections of 5-10mm, uniformly spreading the cynanchum paniculatum decoction pieces in an oven, setting the drying temperature to be not more than 60 ℃, drying in the shade, screening out medicinal scraps by using a sieve with the diameter of a sieve pore of 1mm, fumigating and sterilizing the cynanchum paniculatum decoction pieces for five minutes by using 95% alcohol before placing in the oven, so that the residual alcohol is completely volatilized when the oven is dried;
extracting and concentrating: putting 10kg of cynanchum paniculatum decoction pieces into an extraction tank, adding 500g of beta-cyclodextrin, adding 9 times of water, soaking for 30 minutes, starting hot steam for heating, soaking for 90 minutes at 80 ℃ for the first time, adding 7 times of water for soaking for 60 minutes at 80 ℃ for the second time, filtering decoction by a 300-mesh filter screen, combining filtrates of the two times to obtain an extracting solution, concentrating the extracting solution at 50-80 ℃ under reduced pressure until the relative density is 1.05-1.15, detecting the property of the extract, measuring the solid content, and measuring the paste yield;
spray drying: weighing a proper amount of maltodextrin, adding water for dissolving, mixing the solution with the extract, setting the air inlet temperature to be 180 ℃, controlling the air inlet temperature to be 170-190 ℃ and the air outlet temperature to be 70-95 ℃, and carrying out spray drying to obtain extract powder, wherein the detection characters and the moisture of the extract powder are obtained;
total mixing: weighing an appropriate amount of maltodextrin, mixing with the extract powder to obtain total mixed powder, and detecting the content of the total mixed powder;
and (3) granulating: taking the total mixed powder, and performing dry granulation. And filling the prepared granules into a medical low-density polyethylene bag and sealing for later use. Detecting the characters, the granularity and the moisture of the particles to be packaged;
subpackaging: and (4) operating according to an operation program of the particle racking machine, adjusting the loading quantity and the batch number, packaging the particles to be packaged, and taking samples for finished product inspection.
Example two:
the difference from the first embodiment is that 10kg of cynanchum paniculatum decoction pieces are put into an extraction tank, 400g of beta-cyclodextrin is added, 9 times of water is added, the cynanchum paniculatum decoction pieces are soaked for 30 minutes, hot steam is started to heat, the first 80 ℃ warm soaking is carried out for 90 minutes, 7 times of water is added for the second time, the second 80 ℃ warm soaking is carried out for 60 minutes, decoction is filtered by a 300-mesh filter screen, two times of filtrate is combined to obtain an extracting solution, the extracting solution is subjected to reduced pressure concentration at 50-80 ℃ until the relative density is 1.05-1.15, the properties of the extract are detected, the solid content is measured, and the extract yield is measured and calculated.
Example three:
the difference from the first embodiment is that 10kg of cynanchum paniculatum decoction pieces are put into an extraction tank, 300g of beta-cyclodextrin is added, 9 times of water is added, the cynanchum paniculatum decoction pieces are soaked for 30 minutes, hot steam is started to heat, the first 80 ℃ warm soaking is carried out for 90 minutes, 7 times of water is added for the second time, the second 80 ℃ warm soaking is carried out for 60 minutes, decoction is filtered by a 300-mesh filter screen, two times of filtrate is combined to obtain an extracting solution, the extracting solution is subjected to reduced pressure concentration at 50-80 ℃ until the relative density is 1.05-1.15, the properties of the extract are detected, the solid content is measured, and the extract yield is measured and calculated.
Comparative example: without addition of beta-cyclodextrin
The difference from the first embodiment is that 10kg of cynanchum paniculatum decoction pieces are put into an extraction tank, 9 times of water is added, the cynanchum paniculatum decoction pieces are soaked for 30 minutes, hot steam is started for heating, the first time of soaking is carried out at 80 ℃ for 90 minutes, 7 times of water is added for soaking at 80 ℃ for 60 minutes, decoction is filtered by a 300-mesh filter screen, two times of filtering liquid is combined to obtain extracting solution, the extracting solution is subjected to reduced pressure concentration at 50-80 ℃ until the relative density is 1.05-1.15, the properties of the extract are detected, the solid content is measured, and the extract yield is measured and calculated.
The contents of paeonol in the paniculate swallowwort root formula granules prepared in the first, second and third examples and the comparative example were measured, and the cream yield and transfer rate were calculated, and the results are shown in table 1.
TABLE 1 paniculate swallowwort root formulation example and comparative example results
Figure BDA0003431059850000051
Compared with the results of the comparative example, the first embodiment shows that the beta-cyclodextrin is added for warm soaking together in the extraction process, so that the loss of paeonol can be effectively reduced, and the transfer rate is improved.
As can be seen from the comparison of the results of the first, second and third examples, the paeonol content and the transfer rate increase with the increase of the addition amount of the beta-cyclodextrin.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to those skilled in the art may occur to persons skilled in the art without departing from the spirit and scope of the present invention.

Claims (6)

1. A preparation method of paniculate swallowwort root formula granules is characterized by comprising the following steps:
(1) pretreatment: processing the cynanchum paniculatum medicinal material to obtain cynanchum paniculatum decoction pieces;
(2) extraction: putting the cynanchum paniculatum decoction pieces into an extraction tank, adding a proper amount of beta-cyclodextrin, adding water which is 8-10 times of the material dosage of the cynanchum paniculatum decoction pieces for soaking, starting hot steam for heating, soaking at 70-85 ℃ for 70-90 minutes, filtering decoction liquid through a 300-mesh filter screen to obtain filtrate, adding water which is 6-8 times of the material dosage of the cynanchum paniculatum decoction pieces for soaking at 80 ℃ for 55-65 minutes, filtering the decoction liquid through a 300-mesh filter screen to obtain filtrate, and combining the two filtrates to obtain an extracting solution;
(3) concentration: concentrating the product obtained in the extraction step at 50-80 deg.C under reduced pressure to relative density of 1.05-1.15 to obtain extract;
(4) and (3) drying: weighing a proper amount of maltodextrin, adding water to dissolve the maltodextrin, mixing the solution with the extract, and then performing spray drying, wherein the air inlet temperature is controlled to be 170 ℃ and 190 ℃, and the air outlet temperature is controlled to be 70-95 ℃ to obtain extract powder;
(5) total mixing: weighing appropriate amount of maltodextrin, and mixing with the extract powder to obtain total mixed powder;
(6) and (3) granulating: and taking the total mixed powder, and performing dry granulation to obtain the formula granules.
2. The method for preparing paniculate swallowwort root formula granules according to claim 1, wherein the mass ratio of the paniculate swallowwort root decoction pieces to the beta-cyclodextrin in the extraction step is 15: 1-20: 1.
3. the method for preparing paniculate swallowwort root formulation granules according to claim 1, wherein the extraction step is carried out by using a straight-tube extraction tank, the concentration step is carried out by using a single-effect external circulation concentrator, the drying step is carried out by using a spray dryer, the total mixing step is carried out by using a multi-directional motion mixer, and the granulation step is carried out by using a dry granulator.
4. The method for preparing paniculate swallowwort root granules according to claim 1, wherein the extraction step is carried out by soaking paniculate swallowwort root decoction pieces in beta-cyclodextrin together.
5. The method for preparing the paniculate swallowwort root formula granules according to claim 1, wherein the pre-treatment step comprises removing impurities such as residual stems from the paniculate swallowwort root, washing with water, cutting into 5-10mm short sections on a medicine cutting machine, uniformly spreading the paniculate swallowwort root decoction pieces in an oven, setting the drying temperature not to exceed 60 ℃, drying in the shade, and sieving to remove medicine scraps by a sieve with the diameter of 1 mm.
6. A paniculate swallowwort formulation prepared by the process for preparing a paniculate swallowwort formulation as claimed in any one of claims 1 to 5.
CN202111609313.3A 2021-12-24 2021-12-24 Cynanchum paniculatum formula granules and preparation method thereof Pending CN114129522A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1985856A (en) * 2006-12-05 2007-06-27 谭登平 Method of retaining scent during extracting Chinese medicine component
CN107373271A (en) * 2017-09-18 2017-11-24 四川三匠苦荞科技开发有限公司 Tartary buckwheat beverage and preparation method thereof
CN110227091A (en) * 2019-06-28 2019-09-13 神威药业集团有限公司 The extraction of paniculate swallowwort medicinal ingredient and its granule and preparation method
CN111973655A (en) * 2020-09-10 2020-11-24 广州市香雪制药股份有限公司 Preparation method of fructus cannabis extract
US20210196778A1 (en) * 2018-08-30 2021-07-01 JIANGSU KANION PHARMACEUTICAL Co.,Ltd. Traditional chinese medicine composition and preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1985856A (en) * 2006-12-05 2007-06-27 谭登平 Method of retaining scent during extracting Chinese medicine component
CN107373271A (en) * 2017-09-18 2017-11-24 四川三匠苦荞科技开发有限公司 Tartary buckwheat beverage and preparation method thereof
US20210196778A1 (en) * 2018-08-30 2021-07-01 JIANGSU KANION PHARMACEUTICAL Co.,Ltd. Traditional chinese medicine composition and preparation method and application thereof
CN110227091A (en) * 2019-06-28 2019-09-13 神威药业集团有限公司 The extraction of paniculate swallowwort medicinal ingredient and its granule and preparation method
CN111973655A (en) * 2020-09-10 2020-11-24 广州市香雪制药股份有限公司 Preparation method of fructus cannabis extract

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