CN111991503A - Production process of snake gall and bulbus fritilariae liquid - Google Patents

Production process of snake gall and bulbus fritilariae liquid Download PDF

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CN111991503A
CN111991503A CN202011039873.5A CN202011039873A CN111991503A CN 111991503 A CN111991503 A CN 111991503A CN 202011039873 A CN202011039873 A CN 202011039873A CN 111991503 A CN111991503 A CN 111991503A
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liquid
snake
gall
bulbus fritilariae
production process
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何述金
何承东
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HUNAN XINHUI PHARMACEUTICAL CO Ltd
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HUNAN XINHUI PHARMACEUTICAL CO Ltd
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    • A—HUMAN NECESSITIES
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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
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    • A61K36/88—Liliopsida (monocotyledons)
    • A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
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Abstract

The invention provides a production process of snake bile bulbus fritilariae liquid, which comprises the following steps: step one, crushing fritillary bulb, and extracting to obtain fritillary bulb extract; step two, placing the snake gall into white spirit with the alcohol content of more than 50 percent, sealing and storing, removing gall bladder, collecting the snake gall, mixing the snake gall and the equivalent soaking wine, filtering for the first time, sterilizing and filtering for the second time to obtain a snake gall treatment solution; step three, preparing sucrose into simple syrup; step four, adding purified water into honey, heating, boiling, dissolving, refining until the honey is transparent and clear, filtering, and conveying to a liquid preparation tank; and step five, adding the fritillaria ussuriensis maxim extract, the snake bile treatment liquid and the simple syrup into a liquid preparation tank, stirring, heating to boil, adding the amygdalonitrile solution, uniformly mixing to obtain the snake bile bulbus fritilariae liquid, filling and sterilizing. The snake gall bulbus fritilariae liquid prepared by the production process can ensure the sanitary standard and the clarity requirement, and can effectively expel wind, relieve cough, remove phlegm and dissipate stagnation.

Description

Production process of snake gall and bulbus fritilariae liquid
Technical Field
The invention relates to the technical field of traditional Chinese medicine preparation, in particular to a production process of snake gall bulbus fritilariae liquid.
Background
The snake gall bladder is the gall bladder in which the bile is stored in the body of a snake. All snake gall can be used as medicine. The most effective disease curing method by the snake gall is as follows: clearing away heat and toxic materials, dispelling pathogenic wind, eliminating dampness, improving eyesight, and clearing away heart-fire; especially acute rheumatic arthritis, cough due to lung heat, stomach heat pain, liver heat and conjunctival congestion, skin toxic heat and other patients, and has extremely remarkable curative effect; treating external hemorrhoid with fel Serpentis, and applying to the affected part with oleum Sesami, and the preparation can take effect in two or three days; for pain, parotitis, lymphadenectasis, etc. without ulceration, it can be applied to snake gall to relieve inflammation and pain; scabies, intractable tinea, neurodermatitis and other skin diseases can be treated by applying snake gall on the skin.
Tendril-leaved fritillary bulb, Latin school name: fritillaria cirrhosa is a rare Chinese medicinal material. The herb is recorded in the book of Yunnan materia Medica of Ming Dynasty. It is mainly used for treating cough due to affection of exogenous wind-heat, chronic cough due to lung deficiency, less phlegm, and pharyngoxerosis, and has antitussive, expectorant, blood pressure lowering, and antibacterial effects.
The snake gall bulbus fritilariae liquid is a modern developed formula, is a commonly used famous Chinese patent medicine and is used for treating wind-heat cough, excessive phlegm, asthma, chest distress, unsmooth expectoration or chronic cough. The existing preparation method of the snake gall bulbus fritilariae liquid has the defects of unreasonable processing mode of raw materials, relatively simple preparation process flow and the like, so that the prepared snake gall bulbus fritilariae liquid needs to be improved in aspects of sanitation, clarity and utilization rate of active ingredients of the raw materials.
Disclosure of Invention
In view of the above, the invention aims to provide a production process of a snake bile bulbus fritilariae liquid, and aims to optimize the preparation process and ensure the requirements of sanitary standard and clarity.
Based on the above purpose, the invention provides a production process of snake bile bulbus fritilariae liquid, which comprises the following steps:
step one, crushing fritillary bulb, and extracting to obtain fritillary bulb extract;
step two, placing the snake gall into white spirit with the alcohol content of more than 50 percent, sealing and storing, removing gall bladder, collecting the snake gall, mixing the snake gall and the equivalent soaking wine, filtering for the first time, sterilizing and filtering for the second time to obtain a snake gall treatment solution;
step three, preparing sucrose into simple syrup;
step four, adding purified water into honey, heating, boiling, dissolving, refining until the honey is transparent and clear, filtering, and conveying to a liquid preparation tank;
step five, adding the fritillaria ussuriensis maxim extract, the snake bile treatment liquid and the simple syrup into a liquid preparation tank, stirring, heating to boil, adding the amygdalonitrile solution, mixing uniformly to obtain a snake bile bulbus fritilariae liquid, filling and sterilizing;
wherein, each liter of snake gall bulbus fritilariae liquid comprises 70-80g of fritillaria extract, 8-12g of snake gall treatment liquid, 75-85g of honey, 550-570g of simple syrup and 25-35ml of mandelonitrile solution.
The snake bile contains not only bile acid and other effective components, but also massive mucus, protein, parietal cell, bacteria and other ineffective impurities and foreign matters, and some also contains worm eggs. The snake bile treatment is to adopt filtration-sterilization-filtration to remove impurities and foreign matters, thereby ensuring the sanitation and the clarity of the product.
As an optional implementation form, in the first step, the fritillary bulb extract is prepared by extracting pulverized fritillary bulb with 75-85% ethanol under reflux twice, adding 3-4 times of 75-85% ethanol for the first time, soaking for 30-40min, heating with steam to 80-85 deg.C, extracting for 2-3h, and filtering to obtain the first filtrate; adding 2-2.5 times of 75-85% ethanol, heating to 80-85 deg.C, extracting for 1.5-2 hr, filtering to obtain second filtrate, mixing the first filtrate and the second filtrate, and concentrating at 25 deg.C to obtain fluid extract.
Preferably, in the second step, the mass ratio of the snake gall to the white spirit is 1:1, the sealed storage temperature is not more than 20 ℃, and the storage time is not more than two months.
Preferably, the filtration in step two and step three is performed by using a plate and frame filter. Can effectively filter impurities.
And step three, adding a preservative into the simple syrup, wherein each liter of the snake gall bulbus fritilariae liquid contains 1-1.5g of the preservative. Sodium benzoate is preferably used as the preservative.
Preferably, the sterilization in the fifth step adopts high-temperature sterilization by heating to 100-110 ℃. The mode of high-temperature sterilization is adopted for sterilization, so that the situation that no active bacteria, worm eggs and the like exist in the snake gall bulbus fritilariae liquid is effectively ensured, the sanitary requirement is ensured, and meanwhile, the storage time can be prolonged.
Preferably, in the fifth step, the temperature of the heated and boiled liquid preparation tank is reduced by a refrigerating unit, and when the temperature is reduced to 80 ℃, the mandelonitrile solution is added. By the optimized process steps, the curative effect of the effective components of the snake gall bulbus fritilariae liquid is improved.
Preferably, the liquid preparation tank in the fifth step is further added with menthol after being heated and boiled, and each liter of the snake gall bulbus fritilariae liquid contains 0.1-0.2 g.
Preferably, the fritillaria ussuriensis maxim extract in the step one is prepared by adopting supercritical CO2Extracting and collecting by an extraction method. By using supercritical CO2The extraction method has higher extraction rate than solvent extraction method.
By using supercritical CO2The extraction method for extracting fritillaria ussuriensis extract comprises the steps of crushing fritillaria ussuriensis, then placing the crushed fritillaria ussuriensis into a supercritical extraction kettle, wherein the supercritical extraction kettle is used for extracting fritillaria ussuriensis at the temperature of 30-40 ℃ and CO2The fluid pressure is 25-35 MPa, the flow rate of entrainer ethanol is 0.3-0.4 mL/min, the extraction time is 2-3h, the extract is absorbed by methanol to obtain absorption liquid, wherein after 100g of fritillaria ussuriensis powder is extracted, 20-30 mL of methanol is needed to be used for absorption, the absorption liquid is subjected to AB-8 macroporous resin chromatography, the chromatography speed is two column bed volume flow rates per hour, after the chromatography, the chromatographic column is washed by distilled water until the effluent liquid is colorless, then the chromatographic column is washed by ethanol with the mass percentage concentration of 50% of 2 column bed volumes, the ethanol solution with the gradually increased concentration is used for stage elution, the flow rate is 0.8-1.5mL/min, the eluent is collected to obtain fritillaria ussuriensis eluent, after vacuum concentration, dialysis is carried out for 2-3d, and the fritillaria ussuriensis total alkaloids extract is obtained by freeze-. The concentrations of the ethanol solution in the stage elution are 80%, 90% and 95%. Collecting the eluent refers to collecting the eluent of 90% ethanol solution.
Preferably, the production process further comprises the steps of sequentially performing light inspection and packaging on the filled and sterilized snake gall bulbus fritilariae liquid. The filling adopts a glass bottle for filling, and the purpose of the lamp inspection is to ensure that products after the lamp inspection do not have unqualified products such as insufficient filling amount, untight prick cover, bottle damage, glass chips, floccules, precipitates, coke chips and the like.
The invention has the beneficial effects that:
1. the snake gall bulbus fritilariae liquid prepared by the production process can ensure the sanitary standard and the clarity requirement, can effectively dispel wind, relieve cough, eliminate phlegm and dissipate stagnation, and is used for treating wind-heat cough, excessive phlegm, asthma, chest distress, unsmooth expectoration or chronic cough.
2. By adopting the production process, the ineffective impurities and foreign matters such as mucus, parietal cells, bacteria, worm eggs and the like in the snake gall can be effectively removed.
3. The supercritical extraction can be carried out at the temperature close to room temperature (35-40 ℃) and CO2The gas is extracted under a cover, so that the oxidation and the dissipation of heat-sensitive substances are effectively prevented. Therefore, the effective components of fritillary bulb are kept in the extract. Supercritical CO2The extraction rate of the total alkaloid extracted by fluid is about 93 percent, the extraction rate of the total alkaloid extracted by an ethanol solvent is about 86 percent, and the total alkaloid is extracted by supercritical CO2Fluid extraction methods are preferred over solvent extraction methods.
Detailed Description
To make the objects, technical solutions and advantages of the present disclosure more apparent, the present disclosure is further described in detail below with reference to specific embodiments.
It should be noted that technical terms or scientific terms used in the embodiments of the present specification should have a general meaning as understood by those having ordinary skill in the art to which the present disclosure belongs, unless otherwise defined. The word "comprising" or "comprises", and the like, means that the element or item listed before the word covers the element or item listed after the word and its equivalents, but does not exclude other elements or items.
Example 1
A snake bile and bulbus fritilariae liquid comprises the following components in each liter of the snake bile and bulbus fritilariae liquid:
75g of fritillaria unibracteata extract, 10g of snake bile treatment liquid, 80g of honey, 560g of simple syrup, 30ml of mandelonitrile solution, 1.5g of sodium benzoate and 0.15g of menthol.
The production process of the snake bile bulbus fritilariae liquid comprises the following steps:
step one, crushing fritillary bulb, and extracting to obtain fritillary bulb extract; the Bulbus Fritillariae Ussuriensis extract is prepared by extracting pulverized Bulbus Fritillariae Ussuriensis with 80% ethanol under reflux twice, soaking in 3 times of 80% ethanol for 30-40min, extracting with steam at 80 deg.C for 3 hr, and filtering to obtain first filtrate; adding 2 times of 80% ethanol, heating to 80 deg.C, extracting for 2 hr, filtering to obtain second filtrate, mixing the first filtrate and the second filtrate, and concentrating at 25 deg.C to obtain fluid extract.
And step two, putting the snake gall into the white spirit with the alcohol content of 52 percent, sealing the snake gall and the white spirit by using a plastic barrel, and placing the snake gall and the white spirit in a shade place at the temperature of not more than 20 ℃ to prevent the alcohol from volatilizing. The longest storage time is two months, and the materials are fed into the finished product within two months. When in use, the gall bladder is removed, the gall in the gall bladder is pressed dry, the gall is collected and mixed with the equal amount of wine liquid to prepare liquid, and then the snake gall treatment liquid is obtained after primary filtration, sterilization and secondary filtration; wherein, the filtration adopts a plate-frame filter for filtration, and three layers of filter paper plus one layer of silk cloth/single panel are adopted in the filtration process.
And step three, closing a seabed valve of the sugar melting tank, opening a purified water valve of the sugar melting tank, closing the purified water valve when the purified water is put on the water surface and the stirring paddle is submerged completely, opening a steam valve, heating the purified water to boil, then opening the stirring, opening a vacuum valve, adding cane sugar into the sugar melting tank, heating to fully dissolve the cane sugar, and refining into simple syrup.
And step four, adding honey into a honey mixing tank, adding a proper amount of purified water with the same weight as the honey, heating to boil, fully dissolving, mixing until the mixture is transparent and clear, filtering by using a plate-and-frame filter with two layers of filter paper, and conveying to a liquid preparation tank.
And step five, adding the fritillaria ussuriensis maxim extract, the snake bile treatment liquid and the simple syrup into a liquid preparation tank, stirring, heating to boil, cooling to 80 ℃ by a refrigerating unit, adding the amygdalonitrile solution and the menthol, uniformly mixing to obtain the snake bile bulbus fritilariae liquid, filling, sterilizing, testing by a lamp, and packaging.
Example 2
A snake bile and bulbus fritilariae liquid comprises the following components in each liter of the snake bile and bulbus fritilariae liquid:
70g of fritillary bulb extract, 8g of snake bile treatment liquid, 75g of honey, 550g of simple syrup, 25ml of mandelonitrile solution, 1.3g of sodium benzoate and 0.12g of menthol.
The production process of the snake bile bulbus fritilariae liquid comprises the following steps:
step one, crushing fritillary bulb, and extracting to obtain fritillary bulb extract; the Bulbus Fritillariae Ussuriensis extract adopts supercritical CO2The extraction method comprises pulverizing Bulbus Fritillariae Ussuriensis, and placing into supercritical extraction kettle at 35 deg.C under CO2The fluid pressure is 30MPa, the flow rate of entrainer ethanol is 0.35ml/min, the extraction time is 2.5h, and the extract is concentrated into liquid extract at the temperature of 25 ℃.
And step two, putting the snake gall into the white spirit with the alcohol content of 52 percent, sealing the snake gall and the white spirit by using a plastic barrel, and placing the snake gall and the white spirit in a shade place at the temperature of not more than 20 ℃ to prevent the alcohol from volatilizing. The longest storage time is two months, and the materials are fed into the finished product within two months. When in use, the gall bladder is removed, the gall in the gall bladder is pressed dry, the gall is collected and mixed with the equal amount of wine liquid to prepare liquid, and then the snake gall treatment liquid is obtained after primary filtration, sterilization and secondary filtration; wherein, the filtration adopts a plate-frame filter for filtration, and three layers of filter paper plus one layer of silk cloth/single panel are adopted in the filtration process.
And step three, closing a seabed valve of the sugar melting tank, opening a purified water valve of the sugar melting tank, closing the purified water valve when the purified water is put on the water surface and the stirring paddle is submerged completely, opening a steam valve, heating the purified water to boil, then opening the stirring, opening a vacuum valve, adding cane sugar into the sugar melting tank, heating to fully dissolve the cane sugar, and refining into simple syrup.
And step four, adding honey into a honey mixing tank, adding a proper amount of purified water with the same weight as the honey, heating to boil, fully dissolving, mixing until the mixture is transparent and clear, filtering by using a plate-and-frame filter with two layers of filter paper, and conveying to a liquid preparation tank.
And step five, adding the fritillaria ussuriensis maxim extract, the snake bile treatment liquid and the simple syrup into a liquid preparation tank, stirring, heating to boil, cooling to 80 ℃ by a refrigerating unit, adding the amygdalonitrile solution and the menthol, uniformly mixing to obtain the snake bile bulbus fritilariae liquid, filling, sterilizing, testing by a lamp, and packaging.
Example 3
A snake bile and bulbus fritilariae liquid comprises the following components in each liter of the snake bile and bulbus fritilariae liquid:
75g of fritillaria unibracteata extract, 10g of snake bile treatment liquid, 80g of honey, 560g of simple syrup, 30ml of mandelonitrile solution, 1.5g of sodium benzoate and 0.15g of menthol.
The production process of the snake bile bulbus fritilariae liquid comprises the following steps:
step one, crushing fritillary bulb, and extracting to obtain fritillary bulb extract; the Bulbus Fritillariae Ussuriensis extract adopts supercritical CO2The extraction method comprises pulverizing Bulbus Fritillariae Ussuriensis, and placing into supercritical extraction kettle at 35 deg.C under CO2The fluid pressure is 30MPa, the flow rate of entrainer ethanol is 0.35mL/min, the extraction time is 3h, the extract is absorbed by methanol to obtain absorption liquid, wherein, after 100g of fritillaria ussuriensis powder is extracted, 25mL of methanol is needed to be used for absorption, the absorption liquid is subjected to AB-8 macroporous resin chromatography, the chromatography speed is two column bed volume flow rates per hour, after chromatography, the chromatographic column is washed by distilled water firstly until the effluent liquid is colorless, then the chromatographic column is washed by ethanol with the mass percentage concentration of 50 percent of 2 column bed volumes, and then the ethanol solution with gradually increased concentration is used for stage elution with the flow rate of 1.0mL/min, the eluent is collected to obtain fritillaria ussuriensis eluent, after vacuum concentration, dialysis is carried out for 2d, water is changed for 3 times per day to remove small molecular impurities, and freeze-drying is carried out to obtain the fritillaria. Wherein, the concentration of ethanol solution stage elution is 80%, 90% and 95%. Collecting the eluent refers to collecting the eluent of 90% ethanol solution.
And step two, putting the snake gall into the white spirit with the alcohol content of 52 percent, sealing the snake gall and the white spirit by using a plastic barrel, and placing the snake gall and the white spirit in a shade place at the temperature of not more than 20 ℃ to prevent the alcohol from volatilizing. The longest storage time is two months, and the materials are fed into the finished product within two months. When in use, the gall bladder is removed, the gall in the gall bladder is pressed dry, the gall is collected and mixed with the equal amount of wine liquid to prepare liquid, and then the snake gall treatment liquid is obtained after primary filtration, sterilization and secondary filtration; wherein, the filtration adopts a plate-frame filter for filtration, and three layers of filter paper plus one layer of silk cloth/single panel are adopted in the filtration process.
And step three, closing a seabed valve of the sugar melting tank, opening a purified water valve of the sugar melting tank, closing the purified water valve when the purified water is put on the water surface and the stirring paddle is submerged completely, opening a steam valve, heating the purified water to boil, then opening the stirring, opening a vacuum valve, adding cane sugar into the sugar melting tank, heating to fully dissolve the cane sugar, and refining into simple syrup.
And step four, adding honey into a honey mixing tank, adding a proper amount of purified water with the same weight as the honey, heating to boil, fully dissolving, mixing until the mixture is transparent and clear, filtering by using a plate-and-frame filter with two layers of filter paper, and conveying to a liquid preparation tank.
And step five, adding the fritillaria ussuriensis maxim extract, the snake bile treatment liquid and the simple syrup into a liquid preparation tank, stirring, heating to boil, cooling to 80 ℃ by a refrigerating unit, adding the amygdalonitrile solution and the menthol, uniformly mixing to obtain the snake bile bulbus fritilariae liquid, filling, sterilizing, testing by a lamp, and packaging.
Example 4
A snake bile and bulbus fritilariae liquid comprises the following components in each liter of the snake bile and bulbus fritilariae liquid:
80g of fritillaria unibracteata extract, 12g of snake bile treatment liquid, 85g of honey, 570g of simple syrup, 35ml of mandelonitrile solution, 1.5g of sodium benzoate and 0.18g of menthol.
The production process of the snake bile bulbus fritilariae liquid comprises the following steps:
step one, crushing fritillary bulb, and extracting to obtain fritillary bulb extract; the Bulbus Fritillariae Ussuriensis extract adopts supercritical CO2The extraction method comprises pulverizing Bulbus Fritillariae Ussuriensis, and placing into supercritical extraction kettle at 40 deg.C with CO2The fluid pressure is 35MPa, the flow rate of entrainer ethanol is 0.4ml/min, the extraction time is 2h, the extract is absorbed by methanol to obtain absorption liquid, wherein 100g fritillaria ussuriensis powder is extracted and then is absorbed by 30ml of methanol, the absorption liquid is subjected to AB-8 macroporous resin chromatography, and the chromatography speed is every oneAnd (2) washing the chromatographic column with distilled water after two column bed volume flow rates are carried out for hour, washing the chromatographic column with 2 column bed volumes of 50% ethanol by mass percentage concentration until effluent is colorless, then washing the chromatographic column with gradually increasing concentration of ethanol solution at a flow rate of 1.2mL/min, collecting eluent to obtain fritillaria ussuriensis eluent, carrying out vacuum concentration and dialysis for 2d, changing water for 3 times every day to remove small molecular impurities, and freeze-drying to obtain fritillaria ussuriensis extract mainly containing fritillaria total alkaloids. Wherein, the concentration of ethanol solution stage elution is 80%, 90% and 95%. Collecting the eluent refers to collecting the eluent of 90% ethanol solution.
And step two, putting the snake gall into the white spirit with the alcohol content of 52 percent, sealing the snake gall and the white spirit by using a plastic barrel, and placing the snake gall and the white spirit in a shade place at the temperature of not more than 20 ℃ to prevent the alcohol from volatilizing. The longest storage time is two months, and the materials are fed into the finished product within two months. When in use, the gall bladder is removed, the gall in the gall bladder is pressed dry, the gall is collected and mixed with the equal amount of wine liquid to prepare liquid, and then the snake gall treatment liquid is obtained after primary filtration, sterilization and secondary filtration; wherein, the filtration adopts a plate-frame filter for filtration, and three layers of filter paper plus one layer of silk cloth/single panel are adopted in the filtration process.
And step three, closing a seabed valve of the sugar melting tank, opening a purified water valve of the sugar melting tank, closing the purified water valve when the purified water is put on the water surface and the stirring paddle is submerged completely, opening a steam valve, heating the purified water to boil, then opening the stirring, opening a vacuum valve, adding cane sugar into the sugar melting tank, heating to fully dissolve the cane sugar, and refining into simple syrup.
And step four, adding honey into a honey mixing tank, adding a proper amount of purified water with the same weight as the honey, heating to boil, fully dissolving, mixing until the mixture is transparent and clear, filtering by using a plate-and-frame filter with two layers of filter paper, and conveying to a liquid preparation tank.
And step five, adding the fritillaria ussuriensis maxim extract, the snake bile treatment liquid and the simple syrup into a liquid preparation tank, stirring, heating to boil, cooling to 80 ℃ by a refrigerating unit, adding the amygdalonitrile solution and the menthol, uniformly mixing to obtain the snake bile bulbus fritilariae liquid, filling, sterilizing, testing by a lamp, and packaging.
Comparative example 1
A snake bile and bulbus fritilariae liquid comprises the following components in each liter of the snake bile and bulbus fritilariae liquid:
75g of fritillaria unibracteata extract, 10g of snake bile treatment liquid, 80g of honey, 560g of simple syrup, 30ml of mandelonitrile solution, 1.5g of sodium benzoate and 0.15g of menthol.
The production process of the snake bile bulbus fritilariae liquid comprises the following steps:
step one, crushing fritillary bulb, and extracting to obtain fritillary bulb extract; the Bulbus Fritillariae Ussuriensis extract is prepared by extracting pulverized Bulbus Fritillariae Ussuriensis with 80% ethanol under reflux, adding 3 times of 80% ethanol, soaking for 30min, heating with steam to 80 deg.C, extracting for 3 hr, filtering to obtain filtrate, and concentrating at 25 deg.C to obtain fluid extract.
And step two, putting the snake gall into the white spirit with the alcohol content of 52 percent, sealing the snake gall and the white spirit by using a plastic barrel, and placing the snake gall and the white spirit in a shade place at the temperature of not more than 20 ℃ to prevent the alcohol from volatilizing. The longest storage time is two months, and the materials are fed into the finished product within two months. When in use, the gall bladder is removed, the bile in the gall bladder is pressed dry, the bile is collected and mixed with the equal amount of wine liquid to prepare liquid, and then the liquid is filtered to obtain snake bile treatment liquid; wherein, the filtration adopts a plate-frame filter for filtration, and three layers of filter paper plus one layer of silk cloth/single panel are adopted in the filtration process.
And step three, closing a seabed valve of the sugar melting tank, opening a purified water valve of the sugar melting tank, closing the purified water valve when the purified water is put on the water surface and the stirring paddle is submerged completely, opening a steam valve, heating the purified water to boil, then opening the stirring, opening a vacuum valve, adding cane sugar into the sugar melting tank, heating to fully dissolve the cane sugar, and refining into simple syrup.
And step four, adding honey into a honey mixing tank, adding a proper amount of purified water with the same weight as the honey, heating to boil, fully dissolving, mixing until the mixture is transparent and clear, filtering by using a plate-and-frame filter with two layers of filter paper, and conveying to a liquid preparation tank.
And step five, heating the fritillaria unibracteata extract, the snake bile treatment liquid, the simple syrup and the amygdalonitrile solution in a honey refining tank, conveying the heated fritillaria unibracteata extract, the snake bile and the unibracteal nitrile solution into a liquid preparation tank, uniformly mixing to obtain the snake bile and fritillary bulb liquid, and then filling, inspecting by a lamp and packaging.
The above examples were tested for identification:
(1) taking 40ml of the product, adjusting pH to above 12 with 10% sodium hydroxide solution, extracting with chloroform for 2 times, each time 25ml, and mixing chloroform extractive solutions; adjusting pH of the above water solution to 2, extracting with water saturated n-butanol under shaking for 3 times (20, 10ml), mixing n-butanol extractive solutions, washing with water for 2 times (20, 15ml), collecting n-butanol solution, evaporating in water bath, and dissolving the residue with anhydrous ethanol 1ml to obtain sample solution. Adding ethanol into appropriate amount of snake bile as control medicinal material to obtain solution containing 5mg per 1ml as control medicinal material solution. Adding ethanol into sodium taurocholate as control solution containing 1mg per 1 ml. Performing thin layer chromatography (appendix VI B of the first part of the 1995 edition of Chinese pharmacopoeia), sucking 2 μ l of each of the three solutions, respectively dropping the solution on the same newly prepared silica gel G thin layer plate, placing the plate in a phosphorus pentoxide vacuum drier overnight, developing the plate with toluene-isopropanol-methanol-glacial acetic acid-water (8: 4: 3: 2: 1) as a developing agent, taking out the plate, drying the plate in the air, spraying 10% sulfuric acid ethanol solution, heating the plate at 105 ℃ until the spots are clearly developed, and inspecting the plate under an ultraviolet lamp (365 nm). In the chromatogram of the test solution, fluorescent spots of the same color appear at the positions corresponding to the chromatogram of the reference solution and the chromatogram of the reference solution.
(2) Collecting the chloroform extract of item (1), evaporating to dryness on water bath, and dissolving the residue with 0.5ml of anhydrous ethanol to obtain sample solution. Heating and refluxing another 2g of fritillary bulb reference medicinal material with 80% ethanol for 2 hours, filtering, steaming the filtrate on a water bath till the filtrate is nearly dry, putting the filtrate into a separating funnel, adjusting the filtrate to be alkaline with concentrated ammonia solution, shaking and extracting with chloroform for 2 times, 10ml each time, combining the extracting solutions, steaming the extracting solutions on the water bath, and dissolving the residue with 0.5ml of absolute ethanol to obtain the reference medicinal material solution. According to the test of thin layer chromatography (appendix VI B of the first part of the Chinese pharmacopoeia 1995), 6 mul of each of the two solutions are sucked and respectively spotted on the same silica gel G thin layer plate which takes sodium carboxymethylcellulose as a bonding agent, ethyl acetate-methanol-concentrated ammonia test solution (12: 2: 1) is taken as a developing agent, the solution is developed, taken out, dried in the air and sequentially sprayed with diluted bismuth potassium iodide test solution and sodium nitrite ethanol test solution. Spots of the same color appear on the chromatogram of the test solution at the positions corresponding to those on the chromatogram of the control solution. The result shows that the snake gall bulbus fritilariae liquid prepared by the invention meets the production standard.
By using the extraction rate of total alkaloids as an evaluation index and comparing the superiorities of the two extraction methods, a pre-test result shows that the extraction rate of total alkaloids by an ethanol solvent is about 86 percent, and the supercritical CO extraction2The total alkaloid extraction rate of the fluid extraction is about 93 percent, and the supercritical CO extraction2Fluid extraction methods are preferred over solvent extraction methods.
The experimental test results show that the clarity of the bulbus fritilariae liquid prepared in the example 3 and the example 4 is relatively better, the clarity of the bulbus fritilariae liquid prepared in the example 2 is relatively poorer than that of the bulbus fritilariae liquid prepared in the example 1. The formulation of example 3 is relatively more compatible with the requirements of the production process in terms of extraction purity and extraction yield.
Those of ordinary skill in the art will understand that: the discussion of any embodiment above is meant to be exemplary only, and is not intended to intimate that the scope of the disclosure, including the claims, is limited to these examples; within the idea of the present disclosure, also technical features in the above embodiments or in different embodiments may be combined, steps may be implemented in any order, and there are many other variations of the different aspects of the embodiments of the present description as described above, which are not provided in detail for the sake of brevity.
The embodiments of the present description are intended to embrace all such alternatives, modifications and variances that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalents, improvements, and the like that may be made within the spirit and principles of the embodiments described herein are intended to be included within the scope of the disclosure.

Claims (10)

1. A production process of snake bile bulbus fritilariae liquid is characterized by comprising the following steps:
step one, crushing fritillary bulb, and extracting to obtain fritillary bulb extract;
step two, placing the snake gall into white spirit with the alcohol content of more than 50 percent, sealing and storing, removing gall bladder, collecting the snake gall, mixing the snake gall and the equivalent soaking wine, filtering for the first time, sterilizing and filtering for the second time to obtain a snake gall treatment solution;
step three, preparing sucrose into simple syrup;
step four, adding purified water into honey, heating, boiling, dissolving, refining until the honey is transparent and clear, filtering, and conveying to a liquid preparation tank;
step five, adding the fritillaria ussuriensis maxim extract, the snake bile treatment liquid and the simple syrup into a liquid preparation tank, stirring, heating to boil, adding the amygdalonitrile solution, mixing uniformly to obtain a snake bile bulbus fritilariae liquid, filling and sterilizing;
wherein, each liter of snake gall bulbus fritilariae liquid comprises 70-80g of fritillaria extract, 8-12g of snake gall treatment liquid, 75-85g of honey, 550-570g of simple syrup and 25-35ml of mandelonitrile solution.
2. The production process of the snake bile bulbus fritilariae liquid as claimed in claim 1, wherein the fritillary bulb extract in the first step is prepared by extracting crushed fritillary bulbs with 75-85% ethanol under reflux twice, adding 3-4 times of 75-85% ethanol for the first time, soaking for 30-40min, heating with steam to 80-85 ℃ for extraction for 2-3h, and filtering to obtain the first filtrate; adding 2-2.5 times of 75-85% ethanol, heating to 80-85 deg.C, extracting for 1.5-2 hr, filtering to obtain second filtrate, mixing the first filtrate and the second filtrate, and concentrating at 25 deg.C to obtain fluid extract.
3. The production process of the snake gall and bulbus fritilariae liquid as claimed in claim 1, wherein the mass ratio of snake gall to white spirit in the step two is 1:1, the sealed storage temperature is not more than 20 ℃, and the storage time is not more than two months.
4. The production process of the snake bile bulbus fritilariae liquid as claimed in claim 1, wherein the filtration in the second step and the third step is carried out by adopting a plate and frame filter.
5. The production process of the snake bile bulbus fritilariae liquid as claimed in claim 1, wherein the third step further comprises adding a preservative into the simple syrup, and each liter of the snake bile bulbus fritilariae liquid contains 1-1.5g of the preservative.
6. The production process of the snake bile bulbus fritilariae liquid as claimed in claim 1, wherein the sterilization in the fifth step adopts high-temperature sterilization by heating to 100-110 ℃.
7. The production process of the snake bile bulbus fritilariae liquid as claimed in claim 6, wherein the temperature of the liquid preparation tank after heating and boiling is reduced by a refrigerating unit in the fifth step, and the almond nitrile solution is added when the temperature is reduced to 80 ℃.
8. The production process of the snake gall bulbus fritilariae liquid as claimed in claim 1, wherein menthol is added in the liquid preparation tank in the fifth step after heating and boiling, and each liter of snake gall bulbus fritilariae liquid contains 0.1-0.2 g.
9. The production process of the snake bile Sichuan fritillary bulb liquid as claimed in claim 1, wherein the fritillary bulb extract in the first step is prepared by supercritical CO2Extracting and collecting by an extraction method.
10. The production process of the snake bile bulbus fritilariae liquid as claimed in claim 1, wherein the production process further comprises the steps of sequentially performing lamp inspection and packaging on the filled and sterilized snake bile bulbus fritilariae liquid.
CN202011039873.5A 2020-09-28 2020-09-28 Production process of snake gall and bulbus fritilariae liquid Pending CN111991503A (en)

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Application publication date: 20201127