CN116270955A - Preparation method of flavored wrinkled giant hyssop vital energy oral liquid - Google Patents

Preparation method of flavored wrinkled giant hyssop vital energy oral liquid Download PDF

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CN116270955A
CN116270955A CN202310363385.7A CN202310363385A CN116270955A CN 116270955 A CN116270955 A CN 116270955A CN 202310363385 A CN202310363385 A CN 202310363385A CN 116270955 A CN116270955 A CN 116270955A
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oral liquid
flavored
volatile oil
vital energy
wrinkled giant
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CN116270955B (en
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王峰
黄丽芬
胡丽晖
喻伟红
杨燕欢
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Cspc Jiangxi Golden Lotus Pharmaceutical Co ltd
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    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/532Agastache, e.g. giant hyssop
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    • A61K36/72Rhamnaceae (Buckthorn family), e.g. buckthorn, chewstick or umbrella-tree
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Abstract

The invention discloses a preparation method of flavored wrinkled giant hyssop vital energy oral liquid, which relates to the field of traditional Chinese medicine pharmacy, and comprises the steps of percolating pinellia ternate and radix angelicae by using ethanol as a solvent according to a percolation method of fluid extract, obtaining a percolate, and recovering ethanol; extracting volatile oil from herba Agastaches, atractylodis rhizoma, cortex Magnolia officinalis, pericarpium Citri Tangerinae and folium Perillae by distillation to obtain volatile oil; decocting the residue, poria, radix Platycodi, glycyrrhrizae radix, pericarpium Arecae, fructus Jujubae and rhizoma Zingiberis recens with water for at least three times, mixing decoctions, filtering, concentrating, mixing with percolate, standing, filtering, concentrating, adding sodium benzoate, and cooling to obtain concentrated solution; adding a solubilizing agent polysorbate 80 or a mixture of polysorbate and polyamide-amine dendritic polymer into the volatile oil, adding the mixture into the concentrated solution, and adding water to obtain the product. The invention ensures that the volatile oil and the concentrated solution have good compatibility, greatly improves the clarity of the oral liquid and reduces the possibility of layering.

Description

Preparation method of flavored wrinkled giant hyssop vital energy oral liquid
Technical Field
The invention relates to the field of traditional Chinese medicine pharmacy, in particular to a preparation method of an flavored wrinkled giant hyssop vital energy oral liquid.
Background
The Huoxiang Zhengqi prescription consists of thirteen traditional Chinese medicines of patchouli, perilla leaf, angelica dahurica, stir-fried atractylodes macrocephala, dried orange peel, ginger processed pinellia, ginger processed magnolia bark, poria cocos, platycodon grandiflorum, liquorice, areca peel, jujube and ginger, has the effects of relieving exterior syndrome and eliminating dampness, regulating qi and regulating middle warmer, is mainly used for treating wind cold and internal injury and dampness stagnation, and is a common summer heat relieving medicine in summer. The pharmacological actions of the Chinese medicinal composition mainly comprise stopping vomiting, easing pain, relieving spasm, enhancing cellular immunity and inhibiting bacteria.
However, in the preparation method of the flavored wrinkled giant hyssop vital energy oral liquid, volatile oil is distilled and extracted from patchouli, bighead atractylodes rhizome, magnolia bark, dried orange peel and perilla leaf, the obtained volatile oil is directly added during preparation, the prepared flavored wrinkled giant hyssop vital energy oral liquid can cause the phenomenon that volatile oil floats on the liquid surface and oil marks are attached to the bottle wall during pouring in the long-term storage process, and a small amount of shaking and easy-to-scatter sediment is arranged at the bottom, so that the appearance and clinical curative effect of the product are affected.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art and provides a preparation method of flavored wrinkled giant hyssop vital energy oral liquid.
The technical scheme of the invention is as follows:
a method for preparing an oral liquid containing herba Agastaches for regulating vital energy comprises percolating rhizoma Pinelliae and radix Angelicae Dahuricae with ethanol as solvent to obtain percolate, and recovering ethanol; extracting volatile oil from herba Agastaches, atractylodis rhizoma, cortex Magnolia officinalis, pericarpium Citri Tangerinae and folium Perillae by distillation to obtain volatile oil; decocting the residue, poria, radix Platycodi, glycyrrhrizae radix, pericarpium Arecae, fructus Jujubae and rhizoma Zingiberis recens with water for at least three times, mixing decoctions, filtering, concentrating, mixing with percolate, standing, filtering, concentrating, adding sodium benzoate, and cooling to obtain concentrated solution;
adding a solubilizing agent polysorbate 80 or a mixture of polysorbate and polyamide-amine dendritic polymer into the volatile oil, adding the mixture into the concentrated solution, and adding water to obtain the product.
As a preferable scheme of the invention, the mass ratio of the polysorbate 80 to the volatile oil is 3-10:1.
As a preferred embodiment of the invention, the mass ratio of the polysorbate to the polyamide-amine dendrimer is 1-3:1.
As a preferred embodiment of the present invention, the preparation method of the polyamide-amine type dendritic polymer comprises the following steps: methyl acrylate and ethylenediamine are used as starting monomers, and the preparation method comprises the steps of synthesizing at least 3.5-generation polyamide-amine dendritic polymer, and then purifying.
As a preferred embodiment of the invention, the mixture comprises 1-10wt% of the volatile oil.
As a preferred embodiment of the present invention, the primary filtration is performed by using a ceramic membrane having a pore size of 30 to 60 nm.
As a preferred embodiment of the present invention, the secondary filtration uses nanofiltration membranes with a molecular weight cut-off of 100-300 daltons.
As a preferable scheme of the invention, the volume concentration of the ethanol is 70-90%.
As a preferred embodiment of the present invention, chitosan is further added to the mixture.
The beneficial effects of the invention are as follows:
(1) According to the preparation method of the flavored wrinkled giant hyssop vital energy oral liquid, the tween with a branched structure and the polymer with dendritic macromolecules are added into the volatile oil, so that the linear chain and the dendritic can form a network structure with more cavities, and the hydrophobic and hydrophilic groups are combined on the linear chain and the dendritic, so that the flavored wrinkled giant hyssop vital energy oral liquid has excellent amphipathic property, so that the volatile oil and the concentrated solution have good compatibility, the clarity of the oral liquid is greatly improved, and the layering possibility is reduced.
(2) According to the preparation method of the flavored wrinkled giant hyssop vital energy oral liquid, the chitosan is further added, amino groups on the chitosan have a complexing effect, so that the flocculation sedimentation effect is achieved, and the clarity of the oral liquid is further improved.
Detailed Description
The technical scheme of the invention is further described in the following specific examples.
Tween 80 has the structural formula:
Figure BDA0004165789830000031
the following examples were formulated as follows:
Figure BDA0004165789830000032
example 1
A method for preparing JIAWEIHUANGZHENGQI oral liquid comprises percolating rhizoma Pinelliae and radix Angelicae Dahuricae with 70% (v/v) ethanol as solvent to obtain percolate, and recovering ethanol; extracting volatile oil from herba Agastaches, atractylodis rhizoma, cortex Magnolia officinalis, pericarpium Citri Tangerinae and folium Perillae by distillation to obtain volatile oil; decocting the residue, poria, radix Platycodi, glycyrrhrizae radix, pericarpium Arecae, fructus Jujubae and rhizoma Zingiberis recens with water for three times, the first time for 2 hr, and the second and third times for 1 hr, adding 4 times of water each time, mixing decoctions, filtering, concentrating, mixing with percolate, standing, filtering, concentrating to 1000ml, adding 3g sodium benzoate, and cooling to obtain concentrated solution;
adding polysorbate 80 15g into the volatile oil, adding the mixture into the concentrated solution, and adding water to 1000 ml.
The primary filtration adopts a ceramic membrane with the pore diameter of 45 nm.
The molecular weight cut-off is 200 channels for the secondary filtration.
Example 2
A method for preparing JIAWEIHUANGZHENGQI oral liquid comprises percolating rhizoma Pinelliae and radix Angelicae Dahuricae with 70% (v/v) ethanol as solvent to obtain percolate, and recovering ethanol; extracting volatile oil from herba Agastaches, atractylodis rhizoma, cortex Magnolia officinalis, pericarpium Citri Tangerinae and folium Perillae by distillation to obtain volatile oil; decocting the residue, poria, radix Platycodi, glycyrrhrizae radix, pericarpium Arecae, fructus Jujubae and rhizoma Zingiberis recens with water for three times, the first time for 2 hr, and the second and third times for 1 hr, adding 4 times of water each time, mixing decoctions, filtering, concentrating, mixing with percolate, standing, filtering, concentrating to 1000ml, adding 3g sodium benzoate, and cooling to obtain concentrated solution;
15g of a mixture of polysorbate 80 and a polyamide-amine type dendrimer was added to the volatile oil, and the mixture was added to the concentrated solution, followed by adding water to 1000 ml.
The mass ratio of the polysorbate 80 to the polyamide-amine dendritic polymer is 1:1.
The preparation method of the polyamide-amine dendritic polymer comprises the following steps: dropwise adding Ethylenediamine (EDA) and methanol solution into Methyl Acrylate (MA) in an ice bath salt at the temperature of minus 10 ℃ under the nitrogen atmosphere, reacting for 48 hours with the molar ratio of EDA to MA of 1:5, performing rotary evaporation to obtain 0.5G dendritic molecules, continuously adding 0.5G into the mixed solution of ethylenediamine and methanol, reacting to obtain 1G dendritic molecules, and continuously synthesizing 1G and 2G according to the method until 3.5G dendritic molecules are synthesized.
The primary filtration adopts a ceramic membrane with the pore diameter of 50 nm.
The molecular weight cut-off is 200 channels for the secondary filtration.
Chitosan is also added into the mixture.
Example 3
A method for preparing JIAWEIHUANGZHENGQI oral liquid comprises percolating rhizoma Pinelliae and radix Angelicae Dahuricae with 70% (v/v) ethanol as solvent to obtain percolate, and recovering ethanol; extracting volatile oil from herba Agastaches, atractylodis rhizoma, cortex Magnolia officinalis, pericarpium Citri Tangerinae and folium Perillae by distillation to obtain volatile oil; decocting the residue, poria, radix Platycodi, glycyrrhrizae radix, pericarpium Arecae, fructus Jujubae and rhizoma Zingiberis recens with water for three times, the first time for 2 hr, and the second and third times for 1 hr, adding 4 times of water each time, mixing decoctions, filtering, concentrating, mixing with percolate, standing, filtering, concentrating to 1000ml, adding 3g sodium benzoate, and cooling to obtain concentrated solution;
adding 15g of mixture of polysorbate and polyamide-amine dendritic polymer into the volatile oil, adding the mixture into concentrated solution, and adding water to obtain the product.
The mass ratio of the polysorbate to the polyamide-amine dendritic polymer is 2:1.
The preparation method of the polyamide-amine dendritic polymer comprises the following steps: dropwise adding Ethylenediamine (EDA) and methanol solution into Methyl Acrylate (MA) in an ice bath salt at the temperature of minus 10 ℃ under the nitrogen atmosphere, reacting for 48 hours with the molar ratio of EDA to MA of 1:5, performing rotary evaporation to obtain 0.5G dendritic molecules, continuously adding 0.5G into the mixed solution of ethylenediamine and methanol, reacting to obtain 1G dendritic molecules, and continuously synthesizing 1G and 2G according to the method until 3.5G dendritic molecules are synthesized.
The primary filtration adopts a ceramic membrane with the pore diameter of 45 nm.
The molecular weight cut-off is 250 channels for the secondary filtration.
Example 4
A method for preparing JIAWEIHUANGZHENGQI oral liquid comprises percolating rhizoma Pinelliae and radix Angelicae Dahuricae with 70% (v/v) ethanol as solvent to obtain percolate, and recovering ethanol; extracting volatile oil from herba Agastaches, atractylodis rhizoma, cortex Magnolia officinalis, pericarpium Citri Tangerinae and folium Perillae by distillation to obtain volatile oil; decocting the residue, poria, radix Platycodi, glycyrrhrizae radix, pericarpium Arecae, fructus Jujubae and rhizoma Zingiberis recens with water for three times, the first time for 2 hr, and the second and third times for 1 hr, adding 4 times of water each time, mixing decoctions, filtering, concentrating, mixing with percolate, standing, filtering, concentrating to 1000ml, adding 3g sodium benzoate, and cooling to obtain concentrated solution;
15g of a mixture of polysorbate 80 and a polyamide-amine type dendrimer was added to the volatile oil, and the mixture was added to the concentrated solution, followed by adding water to 1000 ml.
The mass ratio of polysorbate 80 to polyamide-amine dendrimer is 3:1.
The preparation method of the polyamide-amine dendritic polymer comprises the following steps: dropwise adding Ethylenediamine (EDA) and methanol solution into Methyl Acrylate (MA) in an ice bath salt at the temperature of minus 10 ℃ under the nitrogen atmosphere, reacting for 48 hours with the molar ratio of EDA to MA of 1:5, performing rotary evaporation to obtain 0.5G dendritic molecules, continuously adding 0.5G into the mixed solution of ethylenediamine and methanol, reacting to obtain 1G dendritic molecules, and continuously synthesizing 1G and 2G according to the method until 4G dendritic molecules are synthesized.
The primary filtration adopts a ceramic membrane with the pore diameter of 60 nm.
The molecular weight cut-off is 180 channels.
Example 5
A method for preparing JIAWEIHUANGZHENGQI oral liquid comprises percolating rhizoma Pinelliae and radix Angelicae Dahuricae with 70% (v/v) ethanol as solvent to obtain percolate, and recovering ethanol; extracting volatile oil from herba Agastaches, atractylodis rhizoma, cortex Magnolia officinalis, pericarpium Citri Tangerinae and folium Perillae by distillation to obtain volatile oil; decocting the residue, poria, radix Platycodi, glycyrrhrizae radix, pericarpium Arecae, fructus Jujubae and rhizoma Zingiberis recens with water for three times, the first time for 2 hr, and the second and third times for 1 hr, adding 4 times of water each time, mixing decoctions, filtering, concentrating, mixing with percolate, standing, filtering, concentrating to 1000ml, adding 3g sodium benzoate, and cooling to obtain concentrated solution;
15g of a mixture of polysorbate 80 and a polyamide-amine type dendrimer was added to the volatile oil, and the mixture was added to the concentrated solution, followed by adding water to 1000 ml.
The mass ratio of polysorbate 80 to polyamide-amine dendrimer is 3:1.
The preparation method of the polyamide-amine dendritic polymer comprises the following steps: dropwise adding Ethylenediamine (EDA) and methanol solution into Methyl Acrylate (MA) in an ice bath salt at the temperature of minus 10 ℃ under the nitrogen atmosphere, reacting for 48 hours with the molar ratio of EDA to MA of 1:5, performing rotary evaporation to obtain 0.5G dendritic molecules, continuously adding 0.5G into the mixed solution of ethylenediamine and methanol, reacting to obtain 1G dendritic molecules, and continuously synthesizing 1G and 2G according to the method until 4G dendritic molecules are synthesized.
The primary filtration adopts a ceramic membrane with the pore diameter of 60 nm.
The molecular weight cut-off is 180 channels.
1wt% chitosan was also added to the mixture.
Comparative example 1 (Tween 80 free)
A method for preparing JIAWEIHUANGZHENGQI oral liquid comprises percolating rhizoma Pinelliae and radix Angelicae Dahuricae with 70% (v/v) ethanol as solvent to obtain percolate, and recovering ethanol; extracting volatile oil from herba Agastaches, atractylodis rhizoma, cortex Magnolia officinalis, pericarpium Citri Tangerinae and folium Perillae by distillation to obtain volatile oil; decocting the residue, poria, radix Platycodi, glycyrrhrizae radix, pericarpium Arecae, fructus Jujubae and rhizoma Zingiberis recens with water for three times, the first time for 2 hr, and the second and third times for 1 hr, adding 4 times of water each time, mixing decoctions, filtering, concentrating, mixing with percolate, standing, filtering, concentrating to 1000ml, adding 3g sodium benzoate, and cooling to obtain concentrated solution;
15g of a mixture of polyamide-amine type dendritic polymer was added to the volatile oil, and the mixture was added to the concentrated solution, followed by adding water to 1000 ml.
The preparation method of the polyamide-amine dendritic polymer comprises the following steps: dropwise adding Ethylenediamine (EDA) and methanol solution into Methyl Acrylate (MA) in an ice bath salt at the temperature of minus 10 ℃ under the nitrogen atmosphere, reacting for 48 hours with the molar ratio of EDA to MA of 1:5, performing rotary evaporation to obtain 0.5G dendritic molecules, continuously adding 0.5G into the mixed solution of ethylenediamine and methanol, reacting to obtain 1G dendritic molecules, and continuously synthesizing 1G and 2G according to the method until 4G dendritic molecules are synthesized.
The primary filtration adopts a ceramic membrane with the pore diameter of 60 nm.
The molecular weight cut-off is 180 channels.
Comparative example 2 (mixture without tween 80 and dendrimer)
A method for preparing JIAWEIHUANGZHENGQI oral liquid comprises percolating rhizoma Pinelliae and radix Angelicae Dahuricae with 70% (v/v) ethanol as solvent to obtain percolate, and recovering ethanol; extracting volatile oil from herba Agastaches, atractylodis rhizoma, cortex Magnolia officinalis, pericarpium Citri Tangerinae and folium Perillae by distillation to obtain volatile oil; decocting the residue, poria, radix Platycodi, glycyrrhrizae radix, pericarpium Arecae, fructus Jujubae and rhizoma Zingiberis recens with water for three times, the first time for 2 hr, and the second and third times for 1 hr, adding 4 times of water each time, mixing decoctions, filtering, concentrating, mixing with percolate, standing, filtering, concentrating to 1000ml, adding 3g sodium benzoate, and cooling to obtain concentrated solution;
mixing the volatile oil and the concentrated solution, and adding water to 1000 ml.
The primary filtration adopts a ceramic membrane with the pore diameter of 60 nm.
The molecular weight cut-off is 180 channels.
The samples prepared in the examples and comparative examples were packaged on the market, and left for 6 months at a temperature of 40.+ -. 2 ℃ and a relative humidity of 75%.+ -. 5%, and the properties and clarity were examined by sampling at the end of 0 month, 1 month, 2 months, 3 months, 6 months and 9 months, respectively, as shown in Table 1.
Table 1 example and comparative example performance results
Figure BDA0004165789830000081
Figure BDA0004165789830000091
The results show that the performance of the examples is better than the comparative examples, probably for the following reasons: analysis of comparative example 1 shows that by adding tween with branched structure and polymer with dendritic macromolecule into volatile oil, linear chain and dendritic can form network structure with more cavities, and hydrophobic and hydrophilic groups are combined on the network structure, so that the volatile oil and concentrated solution have good compatibility, clarity of oral liquid is greatly improved, and possibility of layering is reduced. Analysis of comparative example 2 shows that the amino group on the chitosan has complexation function, plays a role in flocculation sedimentation, and further improves the clarity of the oral liquid.
The above additional technical features can be freely combined and superimposed by a person skilled in the art without conflict.
The foregoing examples have shown only the preferred embodiments of the invention, which are described in more detail and are not to be construed as limiting the scope of the invention. It should be pointed out that various other corresponding changes and modifications can be made by those skilled in the art in light of the above description of the technical solution and the idea, and all such changes and modifications are intended to be within the scope of the invention as defined in the appended claims.

Claims (9)

1. A preparation method of an oral liquid containing flavored wrinkled giant hyssop and vital energy is characterized in that pinellia ternate and angelica are subjected to diacolation according to a diacolation method of a fluid extract, ethanol is used as a solvent for diacolation, so that a diacolation liquid is obtained, and the ethanol is recovered; extracting volatile oil from herba Agastaches, atractylodis rhizoma, cortex Magnolia officinalis, pericarpium Citri Tangerinae and folium Perillae by distillation to obtain volatile oil; decocting the residue, poria, radix Platycodi, glycyrrhrizae radix, pericarpium Arecae, fructus Jujubae and rhizoma Zingiberis recens with water for at least three times, mixing decoctions, filtering, concentrating, mixing with percolate, standing, filtering, concentrating, adding sodium benzoate, and cooling to obtain concentrated solution;
adding a solubilizing agent polysorbate 80 or a mixture of polysorbate and polyamide-amine dendritic polymer into the volatile oil, adding the mixture into the concentrated solution, and adding water to obtain the product.
2. The method for preparing the flavored wrinkled giant hyssop vital energy oral liquid according to claim 1, wherein the mass ratio of the polysorbate 80 to the volatile oil is 3-10:1.
3. The method for preparing the flavored wrinkled giant hyssop vital energy oral liquid according to claim 1, wherein the mass ratio of the polysorbate to the polyamide-amine dendritic polymer is 1-3:1.
4. The method for preparing the flavored wrinkled giant hyssop vital energy oral liquid according to claim 3, wherein the preparation method of the polyamide-amine dendritic polymer is as follows: methyl acrylate and ethylenediamine are used as starting monomers, and the preparation method comprises the steps of synthesizing at least 3.5-generation polyamide-amine dendritic polymer, and then purifying.
5. The method for preparing the flavored wrinkled giant hyssop vital energy oral liquid according to claim 1, wherein the mixture accounts for 1-10wt% of the volatile oil.
6. The method for preparing the flavored wrinkled giant hyssop vital energy oral liquid according to claim 1, wherein the primary filtering adopts a ceramic membrane with the pore diameter of 30-60 nm.
7. The method for preparing an oral liquid of flavored agastache rugosa as claimed in claim 1, wherein the secondary filtration adopts nanofiltration membrane with molecular weight cut-off of 100-300 daltons.
8. The method for preparing the flavored wrinkled giant hyssop vital energy oral liquid according to claim 1, wherein the volume concentration of the ethanol is 70-90%.
9. The method for preparing an oral liquid of flavored agastache rugosa as claimed in claim 1, wherein chitosan is further added into the mixture.
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Publication number Priority date Publication date Assignee Title
CN103239586A (en) * 2013-05-17 2013-08-14 海南德泽药物研究有限公司 Flavored agastache turbidity-dispelling external preparation as well as preparation method and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103239586A (en) * 2013-05-17 2013-08-14 海南德泽药物研究有限公司 Flavored agastache turbidity-dispelling external preparation as well as preparation method and application thereof

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* Cited by examiner, † Cited by third party
Title
李海兵等: "藿香正气口服液制备工艺改进", 《国际药学研究杂志》, vol. 41, no. 4, pages 490 - 492 *

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