CN110721234B - Preparation method of houttuynia cordata injection for livestock - Google Patents
Preparation method of houttuynia cordata injection for livestock Download PDFInfo
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- CN110721234B CN110721234B CN201911201905.4A CN201911201905A CN110721234B CN 110721234 B CN110721234 B CN 110721234B CN 201911201905 A CN201911201905 A CN 201911201905A CN 110721234 B CN110721234 B CN 110721234B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/78—Saururaceae (Lizard's-tail family)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- 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
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/26—Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0012—Galenical forms characterised by the site of application
- A61K9/0019—Injectable compositions; Intramuscular, intravenous, arterial, subcutaneous administration; Compositions to be administered through the skin in an invasive manner
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/08—Solutions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/12—Antivirals
- A61P31/14—Antivirals for RNA viruses
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/12—Antivirals
- A61P31/14—Antivirals for RNA viruses
- A61P31/16—Antivirals for RNA viruses for influenza or rhinoviruses
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P37/00—Drugs for immunological or allergic disorders
- A61P37/02—Immunomodulators
- A61P37/04—Immunostimulants
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/13—Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
Abstract
The invention discloses a preparation method of a veterinary houttuynia cordata injection, which is characterized in that fresh houttuynia cordata is used as a raw material, 2000 parts by weight of houttuynia cordata is adopted after being cleaned and is crushed and stirred into houttuynia cordata sauce, purified water is added for soaking, a negative pressure distillation technology is adopted, 1000ml of distillate is obtained after distillation, secondary redistillation and tertiary redistillation are carried out in sequence, sodium chloride, benzyl alcohol and polysorbate-80 are added, and the houttuynia cordata injection is obtained after uniform mixing, filtration, encapsulation and sterilization. The preparation method has simple production process and low distillation temperature, overcomes the defects of long time consumption and high distillation temperature of the prior art for producing the houttuynia cordata injection by adopting fresh houttuynia cordata, which causes the oxidation of effective components, and effectively reduces the production cost of the product.
Description
Technical Field
The invention relates to a preparation method of a houttuynia cordata injection for animals, in particular to a preparation method of a houttuynia cordata injection for animals by using fresh whole herb of houttuynia cordata.
Background
The herba Houttuyniae is a herb recorded in Chinese pharmacopoeia, belongs to wild herb of houttuynia of Saururaceae, and is rich in volatile oil, houttuynin, pungent houttuynia cordata alkali and potassium salt. The whole herb is pungent in flavor and cold in nature, and enters lung meridian. Has effects of clearing away heat and toxic materials, relieving swelling, treating sore, promoting urination, removing dampness, clearing heat, relieving dysentery, invigorating stomach, and resolving food stagnation, and can be used for treating lung carbuncle, pyocutaneous disease, hemorrhoid hematochezia, and heat accumulation of spleen and stomach due to excessive heat, toxic heat, dampness, and disease heat. The houttuynia injection is prepared with fresh houttuynia herb and through distillation. Has strong antibacterial effect on hemolytic streptococcus, Staphylococcus aureus, Catalpus coccus, pneumococcus, Escherichia coli, Shigella dysenteriae, and Salmonella typhi. Has inhibitory effect on influenza virus and echovirus. The houttuynia cordata has the antibacterial effect and also has important significance in improving the immunity of the organism. The existing production process has long production period, only the distillation and redistillation processes need 2 days, the production energy consumption is large, and the product cost is high. The effective components of the houttuynia cordata are mainly aldehyde ketone components in the volatile oil, the distillation temperature in the prior art is high, carbonyl groups of the houttuynia cordata are easy to oxidize to generate carboxyl groups, and the carbonyl groups have certain destructive effect on the effective components, so that the extraction rate of the effective components is low, and the production cost is high.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a houttuynia cordata injection for livestock. The preparation method has simple production process and low distillation temperature, overcomes the defects of long time consumption and high distillation temperature of the prior art for producing the houttuynia cordata injection by adopting fresh houttuynia cordata, which causes the oxidation of effective components, and effectively reduces the production cost of the product.
In order to achieve the above purpose, the solution adopted by the invention is as follows:
s1, cleaning: washing fresh herba Houttuyniae, removing silt, impurity and rotten inferior herba Houttuyniae, filtering, transferring to a cutting room, and cutting. Preferably, the elutriation is performed using drinking water or purified water.
S2, soaking: stirring 2000 parts by weight of fresh houttuynia cordata thunb cleaned with S1 with a stirrer to obtain the houttuynia cordata jam.
S3, distillation: transferring the houttuynia cordata jam prepared in the step S2 into an extraction tank, injecting purified water with the weight 2-5 times that of the fresh houttuynia cordata to completely soak the fresh houttuynia cordata, covering the extraction tank, starting the interlayer steam for heating after soaking for 2 hours, starting condensed water after heating to boil, keeping the liquid medicine in a boiling state and collecting distillate for 2 hours for later use, wherein the vacuum degree in the extraction tank is-0.02-0.2 MPa (relative vacuum degree).
S4, secondary redistillation: and (3) placing the distillate prepared in the step (S3) into an extraction tank, covering an upper cover, opening the interlayer for steam heating, heating to boil, then opening cooling water to keep the liquid medicine in a boiling state, and collecting the distillate for 2 hours for later use, wherein the vacuum degree in the extraction tank is-0.02-0.2 MPa (relative vacuum degree).
S5, tertiary redistillation: and (3) placing the distillate prepared in the step (S4) into an extraction tank, covering an upper cover, opening the interlayer for steam heating, heating to boil, then opening cooling water to keep the liquid medicine in a boiling state, and collecting 1000ml of distillate for later use, wherein the vacuum degree in the extraction tank is-0.02-0.2 MPa (relative vacuum degree).
S6, preparing an injection: and (4) transferring the distillate obtained in the step (S5) to a liquid preparation pot, adding 5-8 parts by weight of sodium chloride, 5-15 parts by weight of benzyl alcohol and 1-2.5 parts by weight of polysorbate-80, uniformly mixing, filtering, encapsulating and sterilizing.
Further, the extraction tank is a negative pressure extraction tank, the negative pressure extraction tank is provided with a vacuumizing assembly, vacuumizing can be performed in the extraction tank, the vacuum degree is high, the distillate can be boiled when the temperature in the extraction tank is controlled at a lower level, and damage of high temperature to medicinal components is avoided.
Furthermore, the internal vacuum degree of the extraction tank is-0.05 MPa (relative vacuum degree).
Further, the sodium chloride is 7 parts by weight, the benzyl alcohol is 10 parts by weight, and the polysorbate-80 is 2.5 parts by weight.
The preparation method of the houttuynia cordata injection for livestock provided by the invention has the beneficial effects that:
compared with the prior art, the preparation method of the veterinary houttuynia cordata injection adopts a negative pressure distillation technology, so that the interior of an extraction tank is kept in a negative pressure state, when the extraction tank is heated, a mixture of houttuynia cordata sauce and water is boiled at 60-75 ℃ to generate a large amount of steam, the houttuynia cordata volatile oil is carried with the steam and enters a condensing device, the operation temperature in the production process is low, and the quality of effective components of the houttuynia cordata can be well protected; meanwhile, in a negative pressure state, volatile oil contained in the houttuynia cordata has higher volatility, so that the distillation efficiency is improved, the production time is shortened, and the production energy consumption is favorably reduced, thereby reducing the production cost.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described below with reference to specific examples.
Example 1
The embodiment provides a preparation method of a houttuynia cordata injection for livestock, which comprises the following steps:
s1, cleaning: washing fresh herba Houttuyniae, removing silt, impurity and rotten inferior herba Houttuyniae, filtering, transferring to a cutting room, and cutting. Preferably, the elutriation is performed using drinking water or purified water.
S2, soaking: stirring 2000 parts by weight of fresh houttuynia cordata thunb cleaned with S1 with a stirrer to obtain the houttuynia cordata jam.
S3, distillation: transferring the houttuynia cordata jam prepared in the step S2 to an extraction tank, injecting purified water with the weight 2 times that of the fresh houttuynia cordata to completely soak the fresh houttuynia cordata, covering the extraction tank, soaking for 2 hours, starting interlayer steam to heat, keeping the vacuum degree in the extraction tank at 0.2MPa, heating to boil, starting condensed water, keeping the liquid medicine in a boiling state, and collecting distillate for 2 hours for later use.
S4, secondary redistillation: placing the distillate prepared in S3 in an extraction tank, covering an upper cover, opening interlayer steam for heating, keeping the internal vacuum degree of the extraction tank at 0.2MPa, heating to boil, opening cooling water to keep the liquid medicine in a boiling state, and collecting the distillate for 2 hours for later use.
S5, tertiary redistillation: placing the distillate prepared in S4 in an extraction tank, covering an upper cover, starting interlayer steam for heating, keeping the internal vacuum degree of the extraction tank at 0.2MPa, heating to boil, starting cooling water to keep the liquid medicine in a boiling state, and collecting 1000ml of distillate for later use.
S6, preparing an injection: and (4) transferring the distillate obtained in the step (S5) to a liquid preparation pot, adding 5 parts by weight of sodium chloride, 5 parts by weight of benzyl alcohol and 1 part by weight of polysorbate-80, uniformly mixing, filtering, filling and sealing, and sterilizing.
Example 2
The embodiment provides a preparation method of a houttuynia cordata injection for livestock, which comprises the following steps:
s1, cleaning: washing fresh herba Houttuyniae, removing silt, impurity and rotten inferior herba Houttuyniae, filtering, transferring to a cutting room, and cutting. Preferably, the elutriation is performed using drinking water or purified water.
S2, soaking: stirring 2000 parts by weight of fresh houttuynia cordata thunb cleaned with S1 with a stirrer to obtain the houttuynia cordata jam.
S3, distillation: transferring the houttuynia cordata jam prepared in the step S2 into a multifunctional negative pressure extraction tank, injecting purified water with the weight 3 times that of the fresh houttuynia cordata to completely soak the fresh houttuynia cordata, covering the extraction tank, starting the interlayer steam for heating after soaking for 2 hours, starting condensed water after heating to boil, keeping the liquid medicine in a boiling state, and collecting distillate for 2 hours for later use.
S4, secondary redistillation: placing the distillate prepared in S3 in a multifunctional negative pressure extraction tank, covering the upper cover, opening interlayer steam for heating, heating to boil, opening cooling water to make the medicinal liquid in boiling state, and collecting the distillate for 2 hr.
S5, tertiary redistillation: placing the distillate prepared in S4 in a multifunctional negative pressure extraction tank, covering the upper cover, opening interlayer steam for heating, heating to boil, opening cooling water to make the medicinal liquid in boiling state, and collecting 1000ml of distillate for use.
S6, preparing an injection: and (4) transferring the distillate obtained in the step (S5) to a liquid preparation pot, adding 7 parts by weight of sodium chloride, 10 parts by weight of benzyl alcohol and 2.5 parts by weight of polysorbate-80, uniformly mixing, filtering, filling and sealing, and sterilizing.
Example 3
The embodiment provides a preparation method of a houttuynia cordata injection for livestock, which comprises the following steps:
s1, cleaning: washing fresh herba Houttuyniae, removing silt, impurity and rotten inferior herba Houttuyniae, filtering, transferring to a cutting room, and cutting. Preferably, the elutriation is performed using drinking water or purified water.
S2, soaking: stirring 2000 parts by weight of fresh houttuynia cordata thunb cleaned with S1 with a stirrer to obtain the houttuynia cordata jam.
S3, distillation: transferring the houttuynia cordata jam prepared in the step S2 to a multifunctional negative pressure extraction tank, injecting purified water with the weight 5 times that of the fresh houttuynia cordata to completely soak the fresh houttuynia cordata, covering the extraction tank, starting the interlayer steam for heating after soaking for 2 hours, starting condensed water after heating to boil, keeping the liquid medicine in a boiling state, and collecting distillate for 2 hours for later use.
S4, secondary redistillation: placing the distillate prepared in S3 in a multifunctional negative pressure extraction tank, covering the upper cover, opening interlayer steam for heating, heating to boil, opening cooling water to make the medicinal liquid in boiling state, and collecting the distillate for 2 hr.
S5, tertiary redistillation: placing the distillate prepared in S4 in a multifunctional negative pressure extraction tank, covering the upper cover, opening interlayer steam for heating, heating to boil, opening cooling water to make the medicinal liquid in boiling state, and collecting 1000ml of distillate for use.
S6, preparing an injection: and (4) transferring the distillate obtained in the step (S5) to a liquid preparation pot, adding 7 parts by weight of sodium chloride, 10 parts by weight of benzyl alcohol and 2.5 parts by weight of polysorbate-80, uniformly mixing, filtering, filling and sealing, and sterilizing.
Example 4
The embodiment provides a preparation method of a houttuynia cordata injection for livestock, which comprises the following steps:
s1, cleaning: washing fresh herba Houttuyniae, removing silt, impurity and rotten inferior herba Houttuyniae, filtering, transferring to a cutting room, and cutting. Preferably, the elutriation is performed using drinking water or purified water.
S2, soaking: stirring 2000 parts by weight of fresh houttuynia cordata thunb cleaned with S1 with a stirrer to obtain the houttuynia cordata jam.
S3, distillation: transferring the houttuynia cordata jam prepared in the step S2 into a multifunctional negative pressure extraction tank, injecting purified water with the weight 5 times that of the fresh houttuynia cordata to completely soak the fresh houttuynia cordata, covering the extraction tank, soaking for 2 hours, then starting the interlayer steam heating, heating the extraction tank to the vacuum degree of-0.02 MPa, heating to boil, then starting condensed water to keep the liquid medicine in a boiling state, and collecting distillate for 2 hours for later use.
S4, secondary redistillation: placing the distillate prepared in S3 in a multifunctional negative pressure extraction tank, covering the upper cover, opening interlayer steam for heating to a vacuum degree of-0.02 MPa, heating to boil, opening cooling water to make the medicinal liquid in boiling state, and collecting the distillate for 2 hr.
S5, tertiary redistillation: placing the distillate prepared in S4 in a multifunctional negative pressure extraction tank, covering the upper cover, opening interlayer steam for heating to-0.02 MPa, heating to boil, opening cooling water to make the medicinal liquid in boiling state, and collecting 1000ml of distillate for use.
S6, preparing an injection: and (4) transferring the distillate obtained in the step (S5) to a liquid preparation pot, adding 8 parts by weight of sodium chloride, 15 parts by weight of benzyl alcohol and 2.5 parts by weight of polysorbate-80, uniformly mixing, filtering, filling and sealing, and sterilizing.
(I) effective content test
The contents of alpha-terpineol, methyl-n-nonanone, 4-terpineol and borneol acetate in the veterinary houttuynia cordata injection prepared in the example 1-4 are determined according to the gas chromatography method in the appendix VI E of the 2010 version of the Chinese pharmacopoeia, and the results are shown in table 1.
TABLE 1
The test result shows that: the houttuynia cordata injection for animals prepared in the embodiments 1 to 4 all meet the requirements of the public notice of the quality standard draft of the traditional Chinese medicine injection published by the national pharmacopoeia committee on the houttuynia cordata injection. The lower the vacuum degree in the extraction tank, the higher the content of effective components in the injection, but the larger the multiple of water added in the houttuynia cordata jam during distillation, the lower the content of effective components in the injection. The veterinary houttuynia cordata injection prepared in the embodiment 2 has high contents of alpha-terpineol, methyl n-nonanone, 4-terpineol and borneol acetate, improves the distillation efficiency, shortens the production time to 8 hours, is favorable for reducing the production energy consumption, and thus reduces the production cost. Meanwhile, the extraction tank is kept in a negative pressure state all the time, when the extraction tank is heated, the mixture of the houttuynia cordata jam and water begins to boil at 65 ℃, a large amount of steam is generated, the houttuynia cordata volatile oil is carried with the steam and enters a condensing device, the operation temperature in the production process is low, and the quality of effective components of the houttuynia cordata can be well protected.
(II) accelerated stability test
The veterinary houttuynia cordata injection prepared in example 2 is hermetically packaged in a brown ampoule bottle, stored in a constant-temperature drying oven at 45 ℃ for 6 months, and observed for product properties, transparency, pH value and identification tests at 0 month (when preparation is completed), 1 month, 2 months, 3 months, 4 months, 5 months and 6 months, and the results are shown in table 2.
TABLE 2
The test result shows that after the veterinary houttuynia cordata injection prepared in the embodiment 2 of the invention is stored at 45 ℃ for 6 months, the product properties, transparency, pH value and identification test do not change, and the product performance requirements are completely met, so that the veterinary houttuynia cordata injection prepared in the invention is not easy to discolor and precipitate after being stored for a long time, and has stable effective content and reliable quality.
Claims (1)
1. A preparation method of a houttuynia cordata injection for livestock is characterized by comprising the following steps: s1, cleaning: elutriating fresh herba Houttuyniae with drinking water to remove silt, impurities and rotten and inferior herba Houttuyniae, filtering, transferring to a cutting room, and cutting;
s2, soaking: stirring 2000 parts by weight of fresh houttuynia cordata cleaned by S1 with a stirrer to obtain houttuynia cordata sauce;
s3, distillation: transferring the houttuynia cordata jam prepared in the step S2 into an extraction tank, injecting purified water with the weight 3 times that of the fresh houttuynia cordata to completely soak the fresh houttuynia cordata jam, covering the extraction tank, starting interlayer steam for heating after soaking for 2 hours, starting condensed water after heating to boil, wherein the vacuum degree in the extraction tank is-0.05 MPa, the boiling temperature is 60-75 ℃, keeping the liquid medicine in a boiling state, and collecting distillate for 2 hours for later use; the extraction tank is a negative pressure extraction tank, and the negative pressure extraction tank is provided with a vacuumizing assembly and can vacuumize the extraction tank;
s4, secondary redistillation: placing the distillate prepared in S3 in an extraction tank, covering an upper cover, starting interlayer steam for heating, heating to boil, starting cooling water to keep the liquid medicine in a boiling state, and collecting the distillate for 2 hours for later use;
s5, tertiary redistillation: placing the distillate prepared in S4 into an extraction tank, covering an upper cover, starting interlayer steam for heating, keeping the vacuum degree in the extraction tank at-0.05 MPa, heating to boil, starting cooling water to keep the liquid medicine in a boiling state, and collecting 1000ml of distillate for later use;
s6, preparing an injection: and (4) transferring the distillate obtained in the step (S5) to a liquid preparation pot, adding 7 parts by weight of sodium chloride, 10 parts by weight of benzyl alcohol and 2.5 parts by weight of polysorbate-80, uniformly mixing, filtering, filling and sealing, and sterilizing.
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