CN112294869A - Lingguizhu gan decoction extract and preparation method thereof - Google Patents
Lingguizhu gan decoction extract and preparation method thereof Download PDFInfo
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/06—Fungi, e.g. yeasts
- A61K36/07—Basidiomycota, e.g. Cryptococcus
- A61K36/076—Poria
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- 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)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
- A61K36/284—Atractylodes
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/484—Glycyrrhiza (licorice)
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- 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)
- A61K36/54—Lauraceae (Laurel family), e.g. cinnamon or sassafras
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/50—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
- A61K47/69—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit
- A61K47/6949—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes
- A61K47/6951—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes using cyclodextrin
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- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
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- A61P9/00—Drugs for disorders of the cardiovascular system
- A61P9/04—Inotropic agents, i.e. stimulants of cardiac contraction; Drugs for heart failure
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- 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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- 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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- 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
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Abstract
The invention relates to a poria cocos, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction extract and a preparation method thereof. The preparation method comprises the following steps: mixing ramulus Cinnamomi and/or cortex Cinnamomi with Atractylodis rhizoma, moistening with water, steam distilling, and collecting volatile oil, aromatic water and mixed residue; mixing Glycyrrhrizae radix or/and parched Glycyrrhrizae radix with Poria and the mixed residue, extracting with water, filtering the obtained extractive solution, concentrating, and making into water extract fluid extract; clathrating the volatile oil with the mixed solution of the aromatic water and the cyclodextrin to prepare a clathrated solution; mixing the inclusion liquid with the water extract, drying, and preparing extract powder; and (3) adding pharmaceutically acceptable adjuvants into the extract powder, and mixing. According to the invention, by virtue of the principle of similarity and intermiscibility, the cassia twig and/or the cinnamon which contain much oil co-distill the bighead atractylodes rhizome which contains little oil, the volatile oil extraction is facilitated, and therefore, the consistency of the effective components of the extract of the poria, cassia twig and rhizoma atractylodis macrocephalae decoction and the traditional decoction of the poria, cassia twig and rhizoma atractylodis macrocephalae decoction is improved.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine pharmacy, in particular to a poria cocos, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction extract and a preparation method thereof.
Background
The poria, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction is named as poria, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction, is prepared from poria, cassia twig, rhizoma atractylodis macrocephalae and licorice, is suitable for patients with phlegm retention in the heart, fullness in chest and hypochondrium, blurred vision and deep and wiry pulse, is decocted into the right four flavors, is decocted with six liters of water to obtain three liters, removes dregs, is taken by three warmers and is cured after being convenient for use. Zhang Zhongjing, Ling Gui Zhu gan Tang Fang (Ling Gui Zhu Gan Tang Fang) from jin Kui Yao L ü e, phlegm and fluid retention cough syndrome and treatment, is named Ling Gui Ye Gan Tang Fang, which is composed of Fu Ling Si Shu, Gui Zhi san Liang, Bai Zhu san Liang and gan Lian Di, for treating phlegm and fluid retention in the heart, fullness in the chest and hypochondrium, blurred vision, and Fu Xiao Qi Wei Yin, which is the main reason of Ling Gui Zhu Gan Tang when the patient urinates from childhood, the decoction method is' four flavors on the right, six. The modern prescriptions of the Linggui shugan decoction are as follows: 12g of tuckahoe, 9g of cassia twig, 6g of bighead atractylodes rhizome and 6g of honey-fried licorice root are decocted with water for oral administration, and the prescription proportion still adopts the recipe of tuckahoe, cassia twig, bighead atractylodes rhizome and licorice root in the treatise on typhoid fever and miscellaneous diseases, but the honey-fried licorice root is adopted. Linggui shugan Tang is used to treat chronic heart failure, bronchial asthma and pulmonary emphysema.
The formula of the poria, cassia twig and rhizoma atractylodis sweet soup comprises: poria cocos is capable of inducing diuresis and excreting dampness, invigorating spleen and calming heart, mainly contains beta-pachyman accounting for about 93% of dry weight, and also contains pachymic acid, protein, fat, lecithin, choline, histidine, ergosterol and the like, wherein pachyman is insoluble in water, and other components are soluble in water; ramulus Cinnamomi has effects of inducing sweat, expelling pathogenic factors from muscles, warming and dredging channels, supporting yang, regulating qi-flowing, and regulating blood flow, and mainly contains volatile oil, which mainly contains cinnamaldehyde, phenols, organic acids, polysaccharides, glycosides, coumarins and tannin; wherein the volatile oil is the main material basis for exerting sweating and warming and dredging channels and collaterals; the other ingredients are soluble in water; the largehead atractylodes rhizome has the effects of strengthening spleen and tonifying qi, eliminating dampness and promoting diuresis, suppressing sweating and preventing miscarriage, and mainly contains volatile oil, wherein the volatile oil mainly contains atractylone, atractylol ether, juniper camphor, atractylol lactone and the like, and contains fructose, inulin, largehead atractylodes rhizome polysaccharide, various amino acids, vitamin A components and the like; wherein the volatile oil of Atractylodis rhizoma is the main material basis for eliminating dampness and promoting diuresis; other ingredients are dissolved in water; the liquorice has the effects of tonifying spleen and qi, clearing heat and releasing toxin, eliminating phlegm and stopping cough, relieving spasm and pain and harmonizing the drugs, and mainly contains triterpenes (the potassium and calcium salts of triterpenoid saponin glycyrrhizic acid are glycyrrhizin which is a sweet component of the liquorice), flavonoids, alkaloids, polysaccharides and other components, and all the components can be dissolved in water.
In the decoction, the cassia twig (or/and cinnamon) and the bighead atractylodes rhizome contain volatile components, and in the traditional decoction, the volatile components can be partially dissolved, emulsified and suspended in the decoction and are not easy to escape. However, in the process of preparing the poria cocos, cassia twig and rhizoma glycyrrhizae decoction into modern solid preparation type products such as granules and the like according to the prescription of the poria cocos, cassia twig and rhizoma glycyrrhizae decoction, volatile components are completely lost in the steps of concentration, drying and the like of the extracting solution, and finally the content of the volatile components in the obtained product is obviously lower than that of the traditional decoction, and the curative effect is reduced along with the volatile components. Therefore, the modern pharmaceutical technology generally collects volatile oil by steam distillation or carbon dioxide supercritical method, and then adds the volatile oil back to prepare the modern preparation of the tuckahoe, cinnamon, atractylodes and licorice decoction when preparing the final preparation.
Modern technology such as a preparation method of a cassia twig-containing traditional Chinese medicine composition relates to a preparation method of a poria cocos, cassia twig and rhizoma glycyrrhizae decoction, and the preparation method comprises the steps of adding 6-12 times of water into four medicines contained in the poria cocos, cassia twig and rhizoma glycyrrhizae decoction, soaking for 30-120 min, extracting for 1-3 times, wherein the 1 st time of steam distillation extraction is 1-5 h, and collecting 0.5-2 times of aromatic water for later use; combining the water extract, concentrating under reduced pressure at 60-80 ℃ until the relative density is 1.05-1.15 at the corresponding temperature, filtering the water extract concentrate or centrifuging at high speed of 5000-15000 rpm, or adding 0.5-3 times of ethanol for alcohol precipitation, concentrating the extract or supernatant of the alcohol precipitate under reduced pressure at 50-70 ℃ until the relative density is 1.15-1.30, drying the alcohol precipitate or the centrifugal concentrate after the concentration under reduced pressure in a vacuum drying oven at 50-70 ℃ to obtain dry extract, and crushing to obtain extract powder; and (3) clathrating the aromatic water with beta-cyclodextrin with aromatic water amount of 1/5-1/20 at 40-60 ℃ for 1-3 h under heat preservation and stirring, refrigerating at-4 ℃ for 24h, drying, collecting the clathrate, and mixing the clathrate with the extract powder.
In the modern technology, for example, a compound granule of tuckahoe, cinnamon, atractylodes rhizome and licorice decoction and a preparation method thereof are as follows: weighing 4 parts of raw materials of poria cocos, 3 parts of cassia twig, 3 parts of bighead atractylodes rhizome and 2 parts of honey-fried licorice root according to the weight ratio, respectively carrying out steam distillation on the cassia twig and the bighead atractylodes rhizome to obtain volatile oil components, adding 8-12 times of water into residues of the volatile oil components, the residues, the poria cocos and the honey-fried licorice root for carrying out water extraction, extracting for 1-3 times after 1-2 hours of extraction each time, preparing the extracts into freeze-dried powder, adding auxiliary materials into the freeze-dried powder to prepare granules, and spraying the volatile oil onto the surfaces of the prepared granules to obtain.
However, in the above technology, the volatile components of cinnamon twig (or/and cinnamon) and white atractylodes rhizome are obtained in low amount, so that the volatile components in the obtained product are not consistent with those in the traditional decoction. Therefore, how to increase the content of volatile components in cassia twig and bighead atractylodes rhizome in the process of preparing modern dosage form products such as granules is a problem to be overcome.
Disclosure of Invention
Based on the above, the main purpose of the invention is to provide the extract of the tuckahoe, cinnamon, atractylodes rhizome and licorice decoction and the preparation method thereof, when the extract of the tuckahoe, cinnamon, atractylodes rhizome and licorice decoction prepared by the method is used for preparing modern preparation products, the contents of the volatile components of cassia twig (or/and cinnamon) and bighead atractylodes rhizome are high, and are basically consistent with those of the traditional decoction.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a tuckahoe, cinnamon, rhizoma atractylodis and rhizoma glycyrrhizae decoction extract comprises the following steps:
and (3) distillation: mixing ramulus Cinnamomi and/or cortex Cinnamomi with Atractylodis rhizoma, moistening with water, steam distilling, and collecting volatile oil, aromatic water and mixed residue;
extraction: mixing Glycyrrhrizae radix or/and parched Glycyrrhrizae radix with Poria and the mixed residue, extracting with water, filtering the obtained extractive solution, concentrating, and making into water extract fluid extract;
inclusion: adding cyclodextrin into the aromatic water, fully dissolving, and performing inclusion on the volatile oil to prepare inclusion liquid;
and (3) drying: taking the inclusion liquid and the water extract clear paste, drying and preparing extract powder;
mixing: and (3) adding pharmaceutically acceptable auxiliary materials into the extract powder, and mixing to prepare the extract of the tuckahoe, cassia twig, atractylodes rhizome and licorice decoction.
In one embodiment, the step of distilling comprises: the mass of the water is 0.5-3 times of the sum of the mass of the cassia twig or/and the cinnamon and the mass of the bighead atractylodes rhizome.
In one embodiment, the step of distilling comprises: the steam distillation time is 0.5-3 h.
In one embodiment, the step of distilling comprises: the mass of the aromatic water is 0.5-2 times of the sum of the mass of the cassia twig or/and the cinnamon and the mass of the bighead atractylodes rhizome.
In one embodiment, the step of extracting comprises: the mass of the water is 6-14 times of the sum of the mass of the cassia twig or/and the cinnamon, the mass of the bighead atractylodes rhizome, the mass of the liquorice or/and the fried liquorice and the mass of the poria cocos; or/and the extraction times are 1-2 times, and each time lasts for 0.5-2 hours.
In one embodiment, the step of extracting comprises: the relative density of the water extract clear paste is 1.03-1.15.
In one embodiment, the step of extracting comprises: the temperature adopted for concentration is 50-85 ℃.
In one embodiment, the step of including comprises: the cyclodextrin is selected from at least one of beta-cyclodextrin and hydroxypropyl-beta-cyclodextrin.
In one embodiment, the step of including comprises: the mass of the cyclodextrin is 1/5-1/12 of the mass of the aromatic water.
In one embodiment, the step of including comprises: the inclusion mode adopts grinding inclusion.
In one embodiment, the time period of the grinding inclusion is 0.5-3 h.
In one embodiment, the step of drying comprises: the drying mode adopts spray drying.
In one embodiment, the inlet air temperature of the spray drying is 140-195 ℃, and the outlet air temperature of the spray drying is 60-95 ℃.
In one embodiment, the step of mixing comprises: the pharmaceutic adjuvant is selected from one or a combination of more of dextrin, maltodextrin, starch, soluble starch, lactose, microcrystalline cellulose, stevioside, silicon dioxide and magnesium stearate.
In one embodiment, the decoction comprises the following components in parts by mass: 4 parts of poria cocos, 3 parts of cassia twig or/and cinnamon, 2-3 parts of bighead atractylodes rhizome and 2 parts of liquorice or/and fried liquorice.
In one embodiment, the processing step of the fried licorice comprises: taking liquorice decoction pieces, and frying the liquorice decoction pieces to turn yellow according to a frying method in Chinese pharmacopoeia.
The embodiment of the invention provides the poria cocos, cassia twig, rhizoma atractylodis and licorice root decoction extract obtained by the preparation method.
The beneficial effects of the invention include:
the invention mixes cassia twig (and/or cinnamon) and largehead atractylodes rhizome and then distills the mixture, collects volatile oil, aromatic water and dregs obtained by distillation, then mixes the dregs, tuckahoe and liquorice (and/or fried liquorice) and extracts the mixture by water to prepare extract clear paste, and finally prepares the extract of the tuckahoe, cinnamon, rhizoma atractylodis and licorice decoction by mixing the volatile oil and the extract clear paste which are included by mixed liquid of aromatic water and cyclodextrin and pharmaceutical excipients. According to the invention, by means of the principle of similarity and intermiscibility, the cassia twig (and/or cinnamon) with more oil co-distills the bighead atractylodes rhizome with less oil, so that volatile oil extraction and collection are facilitated, the prepared extract of the poria, cassia twig, cassia bark and bighead atractylodes rhizome has high volatile component content, and a modern preparation prepared from the extract of the poria, cassia twig, rhizoma atractylodis macrocephalae can keep better consistency of effective components with the traditional decoction of the poria, cassia twig, rhizoma atractylodis macrocephalae.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The cinnamon in the poria, cassia twig, rhizoma atractylodis and rhizoma glycyrrhizae decoction can be cassia twig or cinnamon. Gui Zhi is adopted in the original prescription from Shang Han Lun and jin Kui Yao L ü e. Only one of cinnamomum cassia and cinnamomum japonica is recorded in a book of Shennong herbal classic, and the cassia twig is not mentioned; however, even though the ancient prescription recorded in Xin Xiu Ben Cao of Han Tang Dynasty uses mu Gui, or Yun mu Gui, i.e., jin mu Gui and singly named Gui. The cinnamon has the same flower and seed as the fungus cinnamon, is only long in leaves, and is also named as the oyster cinnamon by the large and small branch skins. However, the skin texture of the big branch is coarse and deficient like magnolia, the meat is little and the taste is thin, and the big branch is not as good as the small branch. Small branch skin with much meat, half a roll. The cassia bark, the cassia twig and the cassia bark core are all in common taste and pungent and delicious. The fifth generation of the book Shu Ben Cao says that the name of the book Xie is twig bark, … … is cassia twig, also called cinnamon, the name of cinnamon bark is bark removed, and the name is cinnamon core, which is good at the medicine. Gui Zhi is used in modern prescriptions. The present examples consider them as either bark of Cinnamomum cassia Cassia Presl of Lauraceae.
It is understood that the poria cocos, the cassia twig, the cinnamon, the bighead atractylodes rhizome and the liquorice root in the embodiment of the invention can be prepared into decoction pieces by a preparation method of the decoction pieces under various items of Chinese pharmacopoeia or processed products prepared by further processing the decoction pieces. Taking licorice as an example, the processed product such as prepared licorice, the processing technique includes but is not limited to roasting or parching on fire (for example, parching at 120-210 ℃ for 2-15 minutes until the decoction pieces turn yellow), and stir-frying with honey. Related ancient prescriptions such as: prepared licorice root (prepared) in the original prescription from Shang Han Lun. First, in Qin's period, "Huang Zhi Shi", while gan Cao Zhi Shi until Shen jin Yao Fang of Sun Simiao in Tang Dynasty was mentioned first. The embodiment of the invention considers that the liquorice (roasted) is fried liquorice, and the processing method is clear as follows: the raw materials are stir-fried for 2 to 15 minutes at the temperature of 120 to 210 ℃ until the decoction pieces turn yellow. The licorice in the embodiment of the invention can be the processed product of the licorice decoction pieces, or the licorice decoction pieces can be directly adopted. The following examples illustrate the technical solutions of the present invention by taking licorice root decoction pieces and parched licorice root decoction pieces as examples respectively. A preparation method of a tuckahoe, cinnamon, rhizoma atractylodis and rhizoma glycyrrhizae decoction extract comprises the following steps:
and (3) distillation: mixing ramulus Cinnamomi and/or cortex Cinnamomi with Atractylodis rhizoma, moistening with water, steam distilling, and collecting volatile oil, aromatic water and mixed residue;
extraction: mixing Glycyrrhrizae radix or/and parched Glycyrrhrizae radix with Poria and the mixed residue, extracting with water, filtering the obtained extractive solution, concentrating, and making into water extract fluid extract;
inclusion: adding cyclodextrin into the aromatic water, fully dissolving, and performing inclusion on the volatile oil to prepare inclusion liquid;
and (3) drying: taking the inclusion liquid and the water extract clear paste, drying and preparing extract powder;
mixing: and (3) adding pharmaceutically acceptable auxiliary materials into the extract powder, and mixing to prepare the extract of the tuckahoe, cassia twig, atractylodes rhizome and licorice decoction.
It is understood that the steam distillation method involved in the embodiment of the present invention may be water-proof distillation or semi-water-proof distillation.
Preferably, in the step of distilling: the mass of the water is 0.5-3 times of the sum of the mass of the cassia twig or/and the cinnamon and the mass of the bighead atractylodes rhizome. Further preferably, the mass of the water is 2-3 times of the sum of the mass of the cassia twig or/and the cinnamon and the mass of the bighead atractylodes rhizome.
Preferably, in the step of distilling: the steam distillation time is 0.5-3 h.
Preferably, in the step of distilling: the mass of the aromatic water is 0.5-2 times of the sum of the mass of the cassia twig or/and the cinnamon and the mass of the bighead atractylodes rhizome.
According to the embodiment of the invention, the cassia twig and/or the cinnamon and the bighead atractylodes rhizome are mixed and distilled, so that less aromatic water is obtained, more volatile components are collected, the dosage of cyclodextrin is less during subsequent inclusion, and the corresponding inclusion compound can be obtained only by using a small amount of cyclodextrin, so that the dosage of the preparation is reduced. The aromatic water can be used as a solvent for the cyclodextrin in the subsequent inclusion step. The aromatic water can be used for dissolving cyclodextrin, so that the water consumption of the whole process can be reduced. Meanwhile, a small amount of volatile oil can be dissolved in the aromatic water, and the aromatic water produced by distillation is used in the subsequent steps, so that the retention of the volatile oil is facilitated, and the loss of the volatile oil is reduced. Preferably, in the step of extracting: the mass of the water is 6-14 times of the sum of the mass of the cassia twig or/and the cinnamon, the mass of the bighead atractylodes rhizome, the mass of the liquorice or/and the fried liquorice and the mass of the poria cocos. Further preferably, the mass of the water is 8-11 times of the sum of the mass of the cassia twig or/and the cinnamon, the mass of the bighead atractylodes rhizome, and the mass of the licorice or/and the fried licorice and the mass of the poria cocos.
Preferably, in the step of extracting: the extraction times are 1-2 times, and each time is 0.5-2 hours. Further preferably, the extraction times are 1-2 times, and each time lasts for 1-1.5 hours.
Preferably, in the step of extracting: the relative density of the water extract clear paste is 1.03-1.15. Further preferably, the relative density of the clear paste is 1.05-1.10.
It can be understood that, the concentration according to the embodiment of the present invention, including but not limited to concentration under reduced pressure, may be controlled at a temperature of 50 to 85 ℃. Preferably, the concentration temperature is 60-70 ℃.
Preferably, in the step of including: the cyclodextrin is selected from at least one of beta-cyclodextrin and hydroxypropyl-beta-cyclodextrin.
Preferably, in the step of including: the mass of the cyclodextrin is 1/5-1/12 of the mass of the aromatic water.
It is understood that the inclusion method in the embodiments of the present invention is not particularly limited, for example, grinding inclusion may be adopted, and the inclusion time may be controlled to be 0.5 to 3 hours, for example, 0.5 hour, 1 hour, 3 hours, and the like. Preferably, the inclusion time is 0.8-1.5 h.
It is to be understood that the embodiment of the present invention is not particularly limited to the inclusion, and may include, for example: clathrating the volatile oil with mixed solution of aromatic water and cyclodextrin to obtain clathrate solution, mixing the clathrate solution with part of the water extract fluid extract, and drying; drying the rest water extract; and mixing the products obtained by the two steps of drying. For example, it is also possible to: clathrating the volatile oil with mixed solution of aromatic water and cyclodextrin to obtain clathrate, mixing the clathrate with all the water extract fluid extract, and drying.
It is understood that the drying manner is not limited in the embodiments of the present invention, and in the production practice, a suitable drying manner may be selected according to actual requirements, including but not limited to spray drying or freeze drying. Preferably, the drying is spray drying. Compared with freeze drying, the spray drying has low cost and low energy consumption, and is suitable for industrial production.
Preferably, the air inlet temperature of the spray drying is 140-195 ℃, and the air outlet temperature of the spray drying is 60-95 ℃. Further preferably, the air inlet temperature of the spray drying is 180-190 ℃, and the air outlet temperature of the spray drying is 70-80 ℃.
In the embodiment of the invention, the volatile oil is firstly included by adopting the mixed solution of the aromatic water and the cyclodextrin to prepare the inclusion solution, the inclusion solution is mixed with all the water extract clear paste, and spray drying is carried out to obtain uniform products, so that complicated processes such as collecting the inclusion compound in a refrigeration precipitation mode, drying at low temperature, and then mixing with the extract in an equivalent increasing mode are avoided.
Preferably, in the step of mixing: the pharmaceutic adjuvant is selected from one or a combination of more of dextrin, maltodextrin, starch, soluble starch, lactose, microcrystalline cellulose, stevioside, silicon dioxide and magnesium stearate.
Preferably, the formula of the poria cocos, cassia twig, rhizoma atractylodis macrocephalae and rhizoma glycyrrhizae decoction comprises the following components in parts by mass: 4 parts of poria cocos, 3 parts of cassia twig or/and cinnamon, 2-3 parts of bighead atractylodes rhizome and 2 parts of liquorice or/and fried liquorice.
Preferably, the processing steps of the fried licorice comprise: taking liquorice decoction pieces, and frying the liquorice decoction pieces to turn yellow according to a frying method in Chinese pharmacopoeia.
The embodiment of the invention also provides the poria cocos, cassia twig, rhizoma atractylodis and licorice decoction extract obtained by the preparation method.
The poria cocos, cassia twig, rhizoma atractylodis and licorice decoction extract prepared by the embodiment of the invention can be prepared into any appropriate dosage form including but not limited to granules and the like based on the selection of the types of pharmaceutical excipients.
Because the total amount of the volatile oil in the preparation is difficult to accurately measure by modern detection means, the content level of the volatile oil is represented by the content of a certain component in the volatile oil. The cassia twig (or cinnamon) cinnamaldehyde in the tuckahoe, cinnamon, atractylodes and licorice decoction and the atractylone in the bighead atractylodes rhizome are the components with the largest content ratio in the volatile oil of the two decoction pieces respectively, so the contents of the cinnamaldehyde and the atractylone are selected to compare the benefits of the invention. According to determination, the content of the cinnamaldehyde in the cassia twig decoction pieces used in the examples is 0.089%, the content of the cinnamaldehyde in the cassia twig decoction pieces is 3.1%, and the content of the atractylone in the atractylodes macrocephala decoction pieces is 0.132%.
Example 1: ramulus Cinnamomi, Atractylodis rhizoma, Poria, and Glycyrrhrizae radix
The embodiment provides a preparation method of a poria cocos, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction extract, wherein the preparation method comprises the following steps:
the prescription of the tuckahoe, cinnamon, atractylodes and licorice decoction is as follows: 90g of cassia twig decoction pieces, 60g of bighead atractylodes rhizome decoction pieces, 120g of poria cocos decoction pieces and 60g of liquorice root decoction pieces.
The preparation method of the extract of the tuckahoe, cassia twig, rhizoma atractylodis and licorice decoction comprises the following steps:
(1) mixing ramulus Cinnamomi decoction pieces 90g and Atractylodis rhizoma decoction pieces 60g, adding water 330ml, soaking for 60min, introducing steam for distillation (1.0 hr), and collecting 90ml mixed solution of volatile oil and aromatic water;
(2) adding 120g of poria cocos decoction pieces and 60g of liquorice decoction pieces into the residues obtained after distillation, adding 3300ml of water, decocting for 1.0 hour, and filtering to obtain liquid medicine;
(3) concentrating the medicinal liquid at 65 + -5 deg.C under reduced pressure to obtain fluid extract with relative density of 1.08(65 deg.C);
(4) adding 10g of hydroxypropyl-beta-cyclodextrin (1/8.99 of the weight of aromatic water) into the mixed solution of the volatile oil and the aromatic water, dissolving, grinding and clathrating for 60 minutes, adding the obtained clathrating solution into the concentrated extract, stirring uniformly, and spray drying at the air inlet temperature of 185 ℃ and the air outlet temperature of 75 ℃ to obtain 60.5g of dry powder;
(5) and adding 14.3g of pregelatinized starch, 5g of microcrystalline cellulose, 0.1g of stevioside and 0.1g of magnesium stearate into the dried powder obtained by spraying, and uniformly mixing to obtain 80g of the extract of the poria, cassia, rhizoma atractylodis and rhizoma glycyrrhizae decoction.
Taking a sample of the extract of the decoction of poria, cassia, rhizoma atractylodis and licorice, and measuring the contents of cinnamaldehyde and atractylone, the results are shown in table 1.
Example 2: ramulus Cinnamomi, Atractylodis rhizoma, Poria, and radix Glycyrrhizae Preparata
The embodiment provides a preparation method of a poria cocos, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction extract, wherein the preparation method comprises the following steps:
the prescription of the tuckahoe, cinnamon, atractylodes and licorice decoction is as follows: 90g of cassia twig decoction pieces, 60g of bighead atractylodes rhizome decoction pieces, 120g of poria cocos decoction pieces and 60g of fried liquorice root decoction pieces. The fried licorice root decoction pieces can be obtained by the following process: and (3) taking about 300g of liquorice decoction pieces, and stir-frying for 4 minutes at the material temperature of 200 ℃ until the color turns yellow to obtain the stir-fried liquorice decoction pieces.
The preparation method of the extract of the tuckahoe, cassia twig, rhizoma atractylodis and licorice decoction comprises the following steps:
(1) mixing ramulus Cinnamomi decoction pieces 90g and Atractylodis rhizoma decoction pieces 60g, adding water 450ml, soaking for 90 min, introducing steam for distillation (1.5 hr), and collecting mixed solution of volatile oil and aromatic water 120 ml;
(2) adding 120g of Poria decoction pieces and 60g of parched Glycyrrhrizae radix decoction pieces into the residue after distillation, adding 3600ml of water, decocting for 1.0 hr, filtering to obtain medicinal liquid, adding 2880ml of water into the residue, decocting for 0.5 hr, filtering to obtain medicinal liquid, and mixing the medicinal liquids;
(3) concentrating the obtained medicinal liquid at 65 + -5 deg.C under reduced pressure to obtain fluid extract with relative density of 1.08(65 deg.C);
(4) adding 12g of hydroxypropyl-beta-cyclodextrin (1/9.97 of the weight of aromatic water) into the mixed solution of the volatile oil and the aromatic water, dissolving, grinding and clathrating for 60 minutes, adding the clathrating solution into the concentrated extract, stirring uniformly, and spray drying at the air inlet temperature of 185 ℃ and the air outlet temperature of 75 ℃ to obtain 71.7g of dry powder;
(5) adding maltodextrin 7.0g, stevioside 0.1g and silicon dioxide 1.2g into the spray-dried powder, and mixing uniformly to obtain 80g of the extract of the decoction of poria, cassia, rhizoma atractylodis and licorice.
The content of cinnamaldehyde and atractylone in the extract of the Linggui shugan decoction was measured, and the results are shown in Table 1.
Comparative example 1: traditional decoction of poria cocos, cassia twig, bighead atractylodes rhizome and honey-fried licorice root
According to the decoction method of the decoction formula of tuckahoe, cassia twig, rhizoma atractylodis macrocephalae and liquorice in the treatise on typhoid fever and miscellaneous diseases, 120g of tuckahoe decoction pieces, 90g of cassia twig decoction pieces and 60g of rhizoma atractylodis macrocephalae decoction pieces are taken, 60g of liquorice decoction pieces in example 2 are fried, 2600ml of water is added, the decoction is carried out until the decoction volume is about 1300ml, the fire is removed, the filtration is carried out, and the volume of the filtrate is kept to 1300 ml.
The samples were taken to determine the contents of cinnamaldehyde and atractylone, and the results are shown in Table 1.
Comparative example 2: cassia twig and white atractylodes rhizome oil extraction, tuckahoe and liquorice
(1) Taking 90g of cassia twig decoction pieces, adding 900ml of water, heating and distilling for 4 hours, collecting 0.4ml of cassia twig volatile oil, filtering liquid medicine, and reserving the liquid medicine and dregs of a decoction for later use;
taking 60g of rhizoma atractylodis macrocephalae decoction pieces, adding 600ml of water, heating and distilling for 4 hours, collecting 0.3ml of rhizoma atractylodis macrocephalae volatile oil, and filtering liquid medicine for later use; mixing the above residue with the residue;
(2) adding 120g of poria cocos decoction pieces and 60g of liquorice decoction pieces into the combined medicine residues obtained in the step (1), adding 2640ml of water, decocting for 1.5 hours, and filtering to obtain filtrate for later use; adding 2640ml of water into the obtained medicine residues, decocting for 1.5 hours, filtering, and combining the filtrate with the two liquid medicines obtained in the step (1);
(3) concentrating the liquid medicine obtained in the step (2) under reduced pressure, and freeze-drying the concentrated solution to obtain 77.9g of freeze-dried powder;
(4) the cassia twig volatile oil and the largehead atractylodes rhizome volatile oil are uniformly adsorbed by 2.1g of silicon dioxide and then are uniformly mixed with the freeze-dried powder by an equivalent incremental method to obtain 80g of the extract of the tuckahoe, cinnamon, atractylodes rhizome and licorice decoction.
The content of cinnamaldehyde and atractylone in the extract of the Linggui shugan decoction was measured, and the results are shown in Table 1.
Comparative example 3: co-water distillation of tuckahoe, cassia twig, atractylodes and liquorice
(1) Adding 2640ml of water into 120g of poria cocos decoction pieces, 90g of cassia twig decoction pieces, 60g of bighead atractylodes rhizome decoction pieces and 60g of liquorice decoction pieces, soaking for 60min, heating, distilling and extracting for 3h, collecting 330ml of aromatic water for later use, filtering liquid medicine for later use, adding 2640ml of water into dregs of a decoction, heating, decocting for 1 hour, filtering the liquid medicine, and combining the liquid medicines;
(2) concentrating the medicinal liquid at 70 deg.C under reduced pressure to obtain fluid extract with relative density of 1.10(70 deg.C), drying the concentrated fluid extract in a vacuum drying oven at 60 deg.C to obtain dry extract, and pulverizing to obtain extract powder 65.8 g;
(3) adding 80g of beta-cyclodextrin into aromatic water, preserving heat at 50 ℃, stirring for 3h for inclusion, refrigerating at 4 ℃ for 24h, collecting an inclusion compound, concentrating a supernatant to half amount, refrigerating at 4 ℃ for 24h, collecting 72.9g of the inclusion compound in two times, and uniformly mixing the inclusion compound and extract powder to obtain 138.5g of the extract.
The samples were taken to determine the contents of cinnamaldehyde and atractylone, and the results are shown in Table 1.
TABLE 1 comparison of volatile components of extract of Cinnamomum cassia Presl in prescription
Example 3: cinnamon, white atractylodes rhizome, tuckahoe and liquorice
The embodiment provides a preparation method of a poria cocos, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction extract, wherein the preparation method comprises the following steps:
the prescription of the tuckahoe, cinnamon, atractylodes and licorice decoction is as follows: 90g of cinnamon decoction pieces, 90g of bighead atractylodes rhizome decoction pieces, 120g of tuckahoe decoction pieces and 60g of liquorice decoction pieces.
The preparation method of the extract of the tuckahoe, cassia twig, rhizoma atractylodis and licorice decoction comprises the following steps:
(1) mixing cortex Cinnamomi decoction pieces 90g and Atractylodis rhizoma decoction pieces 90g, adding water 540ml, soaking for 30 min, introducing steam for distillation (1.5 hr), and collecting volatile oil and aromatic water mixed solution 120ml (wherein aromatic water is 112 ml);
(2) adding 120g of poria cocos decoction pieces and 60g of liquorice decoction pieces into the residues obtained after distillation, adding 2880ml of water, decocting for 1.5 hours, and filtering to obtain liquid medicine;
(3) concentrating the medicinal liquid at 65 + -5 deg.C under reduced pressure to obtain fluid extract with relative density of 1.08(65 deg.C);
(4) adding 20g of beta-cyclodextrin into the mixed solution of the volatile oil and the aromatic water, dissolving, grinding and clathrating for 60 minutes, adding the clathrating solution into the concentrated clear paste, stirring uniformly, and spray drying at the air inlet temperature of 185 ℃ and the air outlet temperature of 75 ℃ to obtain 83.6g of dry powder;
(5) adding dextrin 16.2g, stevioside 0.1g and magnesium stearate 0.1g into the dried powder obtained by spraying, and uniformly mixing to obtain 100g of the extract of the poria, cassia, rhizoma atractylodis and rhizoma glycyrrhizae decoction.
The content of cinnamaldehyde and atractylone in the extract of the Linggui shugan decoction was measured, and the results are shown in Table 2.
Example 4: cortex Cinnamomi, Atractylodis rhizoma, Poria, and radix Glycyrrhizae Preparata
The embodiment provides a preparation method of a poria cocos, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction extract, wherein the preparation method comprises the following steps:
the prescription of the tuckahoe, cinnamon, atractylodes and licorice decoction is as follows: 90g of cinnamon decoction pieces, 90g of bighead atractylodes rhizome decoction pieces, 120g of tuckahoe decoction pieces and 60g of fried liquorice decoction pieces in example 2.
The preparation method of the extract of the tuckahoe, cassia twig, rhizoma atractylodis and licorice decoction comprises the following steps:
(1) mixing cortex Cinnamomi decoction pieces 90g and Atractylodis rhizoma decoction pieces 90g, adding water 360ml, soaking for 90 min, introducing steam for distillation (1.5 hr), and collecting mixed solution of volatile oil and aromatic water 120ml (wherein aromatic water is 110 ml);
(2) adding 120g of poria cocos decoction pieces and 60g of fried licorice decoction pieces in example 2 into the distillation residue, adding 2880ml of water, decocting for 1.0 hour, filtering to obtain liquid medicine, adding 2880ml of water into the residue, decocting for 0.5 hour, filtering to obtain liquid medicine, and mixing the liquid medicine;
(3) concentrating the medicinal liquid at 65 + -5 deg.C under reduced pressure to obtain fluid extract with relative density of 1.08(65 deg.C);
(4) adding 20g of hydroxypropyl-beta-cyclodextrin into the mixed solution of the volatile oil and the aromatic water, dissolving, grinding and clathrating for 60 minutes, adding the clathrating solution into the concentrated extract, stirring uniformly, and spray drying at the air inlet temperature of 185 ℃ and the air outlet temperature of 75 ℃ to obtain 93.2g of dry powder;
(5) 6.5g of lactose, 0.1g of stevioside and 0.2g of magnesium stearate are added into the dried powder obtained by spraying, and the mixture is uniformly mixed to obtain 100g of the extract of the tuckahoe, cinnamon, atractylodes and licorice decoction.
The content of cinnamaldehyde and atractylone in the extract of the Linggui shugan decoction was measured, and the results are shown in Table 2.
Example 5: cinnamon, white atractylodes rhizome, tuckahoe and liquorice
This example is a variation of example 3, and provides a linggui zhu gan tang extract and a method for preparing the same, the main variation with respect to example 3 is mainly in the parameter settings of the preparation method. Specifically, the preparation method of the linggui zhu gan tang extract of the embodiment includes the following steps:
(1) mixing cortex Cinnamomi decoction pieces 90g and Atractylodis rhizoma decoction pieces 90g, adding water 540ml, soaking for 30 min, introducing water vapor, distilling for 0.5 hr, and collecting mixed solution of volatile oil and aromatic water 120 ml;
(2) adding 120g of Poria decoction pieces and 60g of Glycyrrhrizae radix decoction pieces into the residue obtained after distillation, adding 2160ml of water, decocting for 0.5 hr, extracting for 2 times, and filtering to obtain medicinal liquid;
(3) concentrating the medicinal liquid at 50 deg.C under reduced pressure to obtain fluid extract with relative density of 1.05;
(4) adding 20g of beta-cyclodextrin into the mixed solution of the volatile oil and the aromatic water, dissolving, grinding and clathrating for 30 minutes, adding the clathrating solution into the concentrated clear paste, stirring uniformly, and spray drying at the air inlet temperature of 140 ℃ and the air outlet temperature of 60 ℃ to obtain 79.8g of dry powder;
(5) adding dextrin 20.0g, steviosin 0.1g, and magnesium stearate 0.1g into the spray dried powder, and mixing to obtain extract 100 g.
The content of cinnamaldehyde and atractylone in the extract of the Linggui shugan decoction was measured, and the results are shown in Table 2.
Example 6: cinnamon, white atractylodes rhizome, tuckahoe and liquorice
This example is a variation of example 3, and provides a linggui zhu gan tang extract and a method for preparing the same, the main variation with respect to example 3 is mainly in the parameter settings of the preparation method. Specifically, the preparation method of the linggui zhu gan tang extract of the embodiment includes the following steps:
(1) mixing cortex Cinnamomi decoction pieces 90g and Atractylodis rhizoma decoction pieces 90g, adding water 540ml, soaking for 30 min, introducing water vapor, distilling for 3 hr, and collecting mixed solution of volatile oil and aromatic water 120 ml;
(2) adding 120g of poria cocos decoction pieces and 60g of liquorice decoction pieces into the residues obtained after distillation, adding 5040ml of water, decocting for 2 hours, extracting for 1 time, and filtering to obtain liquid medicine;
(3) concentrating the medicinal liquid at 85 deg.C under reduced pressure to obtain fluid extract with relative density of 1.15;
(4) adding 20g of beta-cyclodextrin into the mixed solution of the volatile oil and the aromatic water, dissolving, grinding and clathrating for 90 minutes, adding the clathrating solution into the concentrated clear paste, stirring uniformly, and spray drying at an air inlet temperature of 195 ℃ and an air outlet temperature of 95 ℃ to obtain 85.7g of dry powder;
(5) adding dextrin 14.1g, stevioside 0.1g and magnesium stearate 0.1g into the dried powder obtained by spraying, and mixing uniformly to obtain 100g of the extract of the decoction.
The content of cinnamaldehyde and atractylone in the extract of the Linggui shugan decoction was measured, and the results are shown in Table 2.
Comparative example 4: traditional decoction of poria cocos, cinnamon, bighead atractylodes rhizome and honey-fried licorice root
According to the decoction method of the decoction formula of tuckahoe, cassia twig, rhizoma atractylodis macrocephalae and liquorice in the treatise on typhoid fever and miscellaneous diseases, 120g of tuckahoe decoction pieces, 90g of cinnamon decoction pieces and 90g of rhizoma atractylodis macrocephalae decoction pieces are taken, 60g of liquorice decoction pieces in example 2 are fried, 2600ml of water is added, the decoction is carried out until the decoction volume is about 1300ml, the fire is removed, the filtration is carried out, and the volume of the filtrate is kept to 1300 ml.
The samples were taken to determine the contents of cinnamaldehyde and atractylone, and the results are shown in Table 2.
Comparative example 5: cinnamon and white atractylodes rhizome oil extraction, tuckahoe and liquorice
(1) Taking 90g of cinnamon decoction pieces, adding 720ml of water, heating and distilling for 3 hours, collecting 1.8ml of volatile oil, filtering liquid medicine, and reserving the liquid medicine and dregs of a decoction for later use;
taking 90g of rhizoma Atractylodis Macrocephalae decoction pieces, adding 720ml of water, heating and distilling for 3 hours, collecting 0.3ml of volatile oil, filtering the liquid medicine, reserving the liquid medicine, and combining the dregs of decoction with the dregs of cassia twig;
(2) adding 120g of poria cocos decoction pieces and 60g of liquorice decoction pieces into the combined medicine residues obtained in the step (1), adding 2880ml of water, decocting for 1.5 hours, and filtering to obtain filtrate for later use; 2880ml of water is added into the medicine residues, the mixture is decocted for 1.0 hour and filtered, and the filtrate is combined with the two liquid medicines obtained in the step (1);
(3) concentrating the liquid medicine obtained in the step (2) under reduced pressure, and freeze-drying the concentrated solution to obtain 95.0g of freeze-dried powder;
(4) the cassia twig volatile oil and the largehead atractylodes rhizome volatile oil are uniformly adsorbed by 5.0g of silicon dioxide and then are uniformly mixed with the freeze-dried powder by an equivalent incremental method to obtain 100g of the extract of the tuckahoe, cinnamon, atractylodes rhizome and licorice decoction.
The content of cinnamaldehyde and atractylone in the extract of the Linggui shugan decoction was measured, and the results are shown in Table 2.
Comparative example 6: co-water distillation of tuckahoe, cinnamon, atractylodes and liquorice
(1) Soaking 120g of Poria decoction pieces, 90g of ramulus Cinnamomi decoction pieces, 90g of Atractylodis rhizoma decoction pieces and 60g of Glycyrrhrizae radix decoction pieces in 2880ml of water for 60min, heating, distilling and extracting for 3h, collecting 360ml of aromatic water for later use, filtering the medicinal liquid for later use, adding 2640ml of water into the residue, heating and decocting for 1 hr, filtering the medicinal liquid, and mixing the medicinal liquids;
(2) concentrating the medicinal liquid at 75 deg.C under reduced pressure to obtain fluid extract with relative density of 1.15(75 deg.C);
(3) drying the obtained concentrated fluid extract in a vacuum drying oven at 60 deg.C to obtain dry extract, and pulverizing to obtain 86.2g extract powder;
(4) adding 100g of beta-cyclodextrin into aromatic water, preserving heat at 50 ℃, stirring for 3h for inclusion, refrigerating at 4 ℃ for 24h, collecting an inclusion compound, concentrating a supernatant to half amount, refrigerating at 4 ℃ for 24h, collecting 89.9g of the inclusion compound in two times, and uniformly mixing the inclusion compound with extract powder to obtain 176.2g of an extract.
The samples were taken to determine the contents of cinnamaldehyde and atractylone, and the results are shown in Table 2.
Comparative example 7: cinnamon and white atractylodes rhizome oil extraction, tuckahoe and liquorice
This comparative example is a comparative example to example 3, the differences with respect to example 3 mainly comprising: cinnamon and white atractylodes rhizome were distilled separately as in example 3. The comparative example comprises the following specific steps:
(1) taking 90g of cinnamon decoction pieces, adding 270ml of water, heating and distilling, collecting volatile oil and aromatic water, filtering liquid medicine, and reserving the liquid medicine and dregs for later use;
taking 90g of rhizoma Atractylodis Macrocephalae decoction pieces, adding 270ml of water, heating and distilling, collecting volatile oil and aromatic water, filtering the liquid medicine, and mixing the residue with the residue of the above ramulus Cinnamomi;
(2) adding 120g of poria cocos decoction pieces and 60g of liquorice decoction pieces into the residues obtained after distillation, adding 2880ml of water, decocting for 1.5 hours, and filtering to obtain liquid medicine;
(3) combining the liquid medicines obtained in the step (1) and the step (2), and then concentrating the mixture into clear paste with the relative density of 1.08(65 ℃) at 65 +/-5 ℃;
(4) mixing the volatile oil obtained by distilling cinnamon decoction pieces and bighead atractylodes rhizome decoction pieces in the step (1) with aromatic water, adding 20g of beta-cyclodextrin into the obtained mixed solution, dissolving, grinding and clathrating for 60 minutes, adding the clathrating solution into the concentrated clear paste, uniformly stirring, and spray-drying at the air inlet temperature of 185 ℃ and the air outlet temperature of 75 ℃ to obtain 84.9g of dry powder;
(5) adding dextrin 14.9g, stevioside 0.1g and magnesium stearate 0.1g into the dried powder obtained by spraying, and mixing uniformly to obtain 100g of the extract of the decoction.
The content of cinnamaldehyde and atractylone in the extract of the Linggui shugan decoction was measured, and the results are shown in Table 2.
The content of the extract of the formula of the decoction is determined by taking volatile components of cinnamaldehyde and atractylone in the formula of the decoction as evaluation indexes, and is compared with the content of the extract of the formula of the decoction prepared by the traditional decoction of the formula of the decoction and other published technologies.
TABLE 2 comparison of volatile components of extract of cortex Cinnamomi decoction pieces in the recipe
As can be seen from tables 1 and 2, the transfer rates of cinnamaldehyde and atractylone are basically consistent when the extract of poria cocos, cassia bark and atractylodes macrocephala extracted by the method is compared with the traditional decoction, while the transfer rates of the extract of volatile oil extracted from cassia twig (or cinnamon) and atractylodes macrocephala are greatly different when the extract of volatile oil extracted from cassia twig (or cinnamon) and atractylodes macrocephala is compared with the traditional decoction, the transfer rates of the extract prepared by extracting volatile oil by decocting the four medicines are obviously different when the extract is compared with the traditional decoction, and the cyclodextrin dosage is too large.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (17)
1. A preparation method of a poria cocos, cassia twig, rhizoma atractylodis macrocephalae and rhizoma glycyrrhizae decoction extract is characterized by comprising the following steps:
and (3) distillation: mixing ramulus Cinnamomi and/or cortex Cinnamomi with Atractylodis rhizoma, moistening with water, steam distilling, and collecting volatile oil, aromatic water and mixed residue;
extraction: mixing Glycyrrhrizae radix or/and parched Glycyrrhrizae radix with Poria and the mixed residue, extracting with water, filtering the obtained extractive solution, concentrating, and making into water extract fluid extract;
inclusion: adding cyclodextrin into the aromatic water, fully dissolving, and performing inclusion on the volatile oil to prepare inclusion liquid;
and (3) drying: taking the inclusion liquid and the water extract clear paste, drying and preparing extract powder;
mixing: and (3) adding pharmaceutically acceptable auxiliary materials into the extract powder, and mixing to prepare the extract of the tuckahoe, cassia twig, atractylodes rhizome and licorice decoction.
2. The method for preparing the extract of Linggui shugan Tang as claimed in claim 1, wherein the distilling step comprises: the mass of the water is 0.5-3 times of the sum of the mass of the cassia twig or/and the cinnamon and the mass of the bighead atractylodes rhizome.
3. The method for preparing the extract of Linggui shugan Tang as claimed in claim 1, wherein the distilling step comprises: the steam distillation time is 0.5-3 h.
4. The method for preparing the extract of Linggui shugan Tang as claimed in any one of claims 1 to 3, wherein the distilling step comprises: the mass of the aromatic water is 0.5-2 times of the sum of the mass of the cassia twig or/and the cinnamon and the mass of the bighead atractylodes rhizome.
5. The method for preparing the extract of Linggui shugan Tang as claimed in any one of claims 1 to 3, wherein the extraction step comprises: the mass of the water is 6-14 times of the sum of the mass of the cassia twig or/and the cinnamon, the mass of the bighead atractylodes rhizome, the mass of the liquorice or/and the fried liquorice and the mass of the poria cocos; or/and the extraction times are 1-2 times, and each time lasts for 0.5-2 hours.
6. The method for preparing the extract of Linggui shugan Tang as claimed in any one of claims 1 to 3, wherein the extraction step comprises: the relative density of the water extract clear paste is 1.03-1.15.
7. The method for preparing the extract of Linggui shugan Tang as claimed in any one of claims 1 to 3, wherein the extraction step comprises: the temperature adopted for concentration is 50-85 ℃.
8. The method for preparing the extract of Linggui shugan Tang as claimed in any one of claims 1 to 3, wherein the inclusion step comprises: the cyclodextrin is selected from at least one of beta-cyclodextrin and hydroxypropyl-beta-cyclodextrin.
9. The method for preparing the extract of Linggui shugan Tang as claimed in any one of claims 1 to 3, wherein the inclusion step comprises: the mass of the cyclodextrin is 1/5-1/12 of the mass of the aromatic water.
10. The method for preparing the extract of Linggui shugan Tang as claimed in any one of claims 1 to 3, wherein the inclusion step comprises: the inclusion mode adopts grinding inclusion.
11. The method for preparing the extract of Linggui shugan Tang as claimed in claim 10, wherein the time period of the grinding inclusion is 0.5-3 h.
12. The method for preparing the extract of Linggui shugan Tang as claimed in any one of claims 1 to 3, wherein the drying step comprises: the drying mode adopts spray drying.
13. The method for preparing the extract of Linggui shugan Tang as claimed in claim 12, wherein the temperature of the inlet air for spray drying is 140-195 ℃ and the temperature of the outlet air for spray drying is 60-95 ℃.
14. The method for preparing the extract of Linggui shugan Tang as claimed in any one of claims 1 to 3, wherein the mixing step comprises: the pharmaceutic adjuvant is selected from one or a combination of more of dextrin, maltodextrin, starch, soluble starch, lactose, microcrystalline cellulose, stevioside, silicon dioxide and magnesium stearate.
15. The method for preparing the extract of the Linggui shugan decoction according to any one of claims 1 to 3, wherein the formula of the Linggui shugan decoction comprises the following components in parts by mass: 4 parts of poria cocos, 3 parts of cassia twig or/and cinnamon, 2-3 parts of bighead atractylodes rhizome and 2 parts of liquorice or/and fried liquorice.
16. The method for preparing the extract of Linggui shugan Tang as claimed in any one of claims 1 to 3, wherein the processing step of the parched licorice root comprises: taking liquorice decoction pieces, and frying the liquorice decoction pieces to turn yellow according to a frying method in Chinese pharmacopoeia.
17. The extract of linggui zhu gan tang obtained by the process of any one of claims 1 to 16.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113230309A (en) * | 2021-05-13 | 2021-08-10 | 广东一方制药有限公司 | Ephedra-cassia twig pair traditional Chinese medicine formula granule and preparation method thereof |
| CN114561248A (en) * | 2022-03-02 | 2022-05-31 | 华润三九（雅安）药业有限公司 | Preparation method and device of volatile oil, inclusion compound and preparation method of pharmaceutical composition |
| CN114632099A (en) * | 2022-03-02 | 2022-06-17 | 华润三九（雅安）药业有限公司 | Preparation method of volatile oil, inclusion compound and preparation method of pharmaceutical composition |
| CN114931593A (en) * | 2021-06-15 | 2022-08-23 | 广西昆泽药业有限公司 | Preparation process of cinnamon formula granule volatile oil inclusion compound |
| CN115737703A (en) * | 2022-11-18 | 2023-03-07 | 安徽中医药大学 | Heart-benefiting particle for treating heart failure and preparation method and application thereof |
| CN115944667A (en) * | 2022-12-29 | 2023-04-11 | 江中药业股份有限公司 | Lingguizhu gan decoction extract and preparation method thereof |
| CN115957254A (en) * | 2023-01-17 | 2023-04-14 | 嘉实（湖南）医药科技有限公司 | Preparation method of poria cocos, cassia twig, rhizoma atractylodis and rhizoma glycyrrhizae decoction granules |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104845737A (en) * | 2014-02-17 | 2015-08-19 | 天士力制药集团股份有限公司 | Extraction method for volatile oil in radix bupleuri |
| CN108653387A (en) * | 2018-06-26 | 2018-10-16 | 安徽中医药大学 | Linggui zhugan decoction compound granule and preparation method thereof |
-
2020
- 2020-10-19 CN CN202011118011.1A patent/CN112294869B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104845737A (en) * | 2014-02-17 | 2015-08-19 | 天士力制药集团股份有限公司 | Extraction method for volatile oil in radix bupleuri |
| CN108653387A (en) * | 2018-06-26 | 2018-10-16 | 安徽中医药大学 | Linggui zhugan decoction compound granule and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王春民等: "二次蒸馏-萃取耦合法提取颈复康制剂挥发油的研究", 《中成药》 * |
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| CN113230309A (en) * | 2021-05-13 | 2021-08-10 | 广东一方制药有限公司 | Ephedra-cassia twig pair traditional Chinese medicine formula granule and preparation method thereof |
| CN114931593A (en) * | 2021-06-15 | 2022-08-23 | 广西昆泽药业有限公司 | Preparation process of cinnamon formula granule volatile oil inclusion compound |
| CN114561248A (en) * | 2022-03-02 | 2022-05-31 | 华润三九（雅安）药业有限公司 | Preparation method and device of volatile oil, inclusion compound and preparation method of pharmaceutical composition |
| CN114632099A (en) * | 2022-03-02 | 2022-06-17 | 华润三九（雅安）药业有限公司 | Preparation method of volatile oil, inclusion compound and preparation method of pharmaceutical composition |
| CN115737703A (en) * | 2022-11-18 | 2023-03-07 | 安徽中医药大学 | Heart-benefiting particle for treating heart failure and preparation method and application thereof |
| CN115944667A (en) * | 2022-12-29 | 2023-04-11 | 江中药业股份有限公司 | Lingguizhu gan decoction extract and preparation method thereof |
| CN115944667B (en) * | 2022-12-29 | 2023-09-22 | 江中药业股份有限公司 | Poria, cassia bark, rhizoma atractylodis and sweet soup extract and preparation method thereof |
| CN115957254A (en) * | 2023-01-17 | 2023-04-14 | 嘉实（湖南）医药科技有限公司 | Preparation method of poria cocos, cassia twig, rhizoma atractylodis and rhizoma glycyrrhizae decoction granules |
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