CN114097965A - Preparation method of bitter beverage for relieving pulmonary fibrosis - Google Patents

Preparation method of bitter beverage for relieving pulmonary fibrosis Download PDF

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Publication number
CN114097965A
CN114097965A CN202111439198.XA CN202111439198A CN114097965A CN 114097965 A CN114097965 A CN 114097965A CN 202111439198 A CN202111439198 A CN 202111439198A CN 114097965 A CN114097965 A CN 114097965A
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limonin
water
pectin
glass bottle
citrus
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廖劲松
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Limeng Qingyuan Biotechnology Co ltd
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Limeng Qingyuan Biotechnology Co ltd
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    • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
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    • A23L2/04—Extraction of juices
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/52—Adding ingredients
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
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    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/231—Pectin; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/33—Heterocyclic compounds
    • A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
    • A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
    • A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline 
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/56—Compounds containing cyclopenta[a]hydrophenanthrene ring systems; Derivatives thereof, e.g. steroids
    • A61K31/58—Compounds containing cyclopenta[a]hydrophenanthrene ring systems; Derivatives thereof, e.g. steroids containing heterocyclic rings, e.g. danazol, stanozolol, pancuronium or digitogenin
    • A61K31/585—Compounds containing cyclopenta[a]hydrophenanthrene ring systems; Derivatives thereof, e.g. steroids containing heterocyclic rings, e.g. danazol, stanozolol, pancuronium or digitogenin containing lactone rings, e.g. oxandrolone, bufalin
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00—Drugs for disorders of the respiratory system
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P11/00—Drugs for disorders of the respiratory system
    • A61P11/04—Drugs for disorders of the respiratory system for throat disorders
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
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Abstract

The invention discloses a preparation method of a bitter beverage for relieving pulmonary fibrosis, which comprises the following steps: cleaning fresh fructus Citri Limoniae, drying, peeling, removing seeds, squeezing, filtering with 150 mesh filter cloth, removing residue, and collecting lemon juice; adding citrus flavone, limonin and pectin into lemon juice, adding water and honey, blending, and homogenizing the blended beverage; the invention can solve the problem that the traditional antiviral drugs have large toxic and side effects or are easy to generate drug resistance by applying the limonin and the citrus flavonoid compounds to the functional beverage, and pectin can prolong the retention time of the limonin and the citrus flavonoid in the throat so as to fully exert the efficacy, increase the actual effects of the limonin and the citrus flavonoid and ensure that the bitter beverage has stronger efficacy of relieving the pulmonary fibrosis.

Description

Preparation method of bitter beverage for relieving pulmonary fibrosis
Technical Field
The invention relates to the field of preparation methods of bitter beverages for relieving pulmonary fibrosis, and particularly relates to a preparation method of bitter beverages for relieving pulmonary fibrosis.
Background
Pulmonary fibrosis is the terminal change of a large group of lung diseases characterized by fibroblast proliferation and massive extracellular matrix aggregation with inflammatory injury and tissue structure destruction, namely structural abnormality caused by abnormal repair after normal alveolar tissues are damaged. The causes of most patients with pulmonary fibrosis are unknown, and the group of diseases is called idiopathic interstitial pneumonia, which is a large group of interstitial lung diseases. The most common disease type with pulmonary fibrosis lesion as the main manifestation form in idiopathic interstitial pneumonia is idiopathic pulmonary fibrosis, which is a serious interstitial lung disease that can cause progressive loss of lung function. Pulmonary fibrosis seriously affects the respiratory function of human body, manifested as dry cough and progressive dyspnea, and the respiratory function of patients is continuously worsened with the aggravation of illness and lung injury.
In the prior art, the retention time of limonin and citrus flavone in the throat of the existing bitter drink is short, so that the efficacy of the bitter drink is weak, and the working efficiency of the limonin and the citrus flavone is reduced, so that a preparation method of the bitter drink for relieving pulmonary fibrosis is needed.
Disclosure of Invention
The present invention aims to provide a method for preparing a bitter beverage for alleviating pulmonary fibrosis, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a bitter beverage for relieving pulmonary fibrosis comprises the following steps:
step one, taking fresh lemons, cleaning, drying, peeling, removing seeds, juicing, filtering by using 150-mesh filter cloth, removing residues, and collecting lemon juice;
adding the citrus flavone, the limonin and the pectin into the lemon juice, adding water and honey for blending, and homogenizing the blended beverage;
and step three, filling the homogenized pulp into a sterilized glass bottle, sealing the glass bottle, sterilizing the glass bottle for 15-20 min at 85-86 ℃, and finally cooling the glass bottle to room temperature to obtain the bitter beverage, wherein the bitter beverage is rich in water-soluble fibers.
Preferably, the purification method of the citrus flavone comprises the following steps:
step one, cleaning and crushing citrus peel, putting the crushed citrus peel and 50-95 v/v% ethanol water solution in an extractor according to the weight ratio of 1: 1-5, extracting for 0.5-1 hour under the reflux state, filtering, and repeating the step for 3 times;
step two, combining the filtered filtrates, concentrating to obtain a citrus peel extract, suspending the obtained citrus peel extract in water, and performing centrifugal filtration to obtain a clear filtrate;
step three, flowing the clear filtrate through an adsorption column filled with pretreated polystyrene type adsorption resin with the granularity of 0.3-1.25 mm at the flow rate of 1.5-8 BV/h at the temperature of 20-30 ℃, wherein the diameter of the adsorption column is as follows: the height ratio is 1: 3-30;
step four, water flows through the adsorption column at the flow rate of 5-10 BV/h; and finally, flowing methanol through the adsorption column at the flow rate of 2-10 BV/h, collecting the obtained liquid, and concentrating to obtain the citrus flavonoid.
Preferably, the purification method of limonin comprises the following steps:
step one, drying and crushing sweet orange seeds, thoroughly degreasing the sweet orange seeds for 24 hours by using petroleum ether (60-90 ℃) in a Soxhlet extractor, extracting the sweet orange seeds for 6 hours by using acetone, concentrating an acetone extracting solution under reduced pressure to dryness, dissolving the acetone extracting solution by using dichloromethane and filtering;
adding isopropanol with 2 times of volume into a dichloromethane solution, uniformly mixing, placing in a refrigerator at 4 ℃, and precipitating a flaky crystal;
step three, recrystallizing the obtained crystal I for 3 times according to the solvent system for determination, evaporating the crystallized mother liquor to dryness, and performing silica gel column chromatography to 100-200 meshes, wherein the eluent is ethyl acetate: methanol 95: 5, detecting with silica gel G thin layer chromatography plate, spraying Ehrlich reagent, mixing the components with the same red spot shift value, and limonin crystal.
Preferably, the pectin purification method comprises the following steps:
step one, soaking lemon peel and squeezed pomace in clear water for half an hour, heating to 90 ℃ for 5 minutes, pressing to remove juice, and rinsing with clear water for several times, so that most of glucoside, pigment and other impurities can be removed, and most of bitter taste is removed;
step two, pouring the ground raw materials into an extraction pot, adding 4 times of water, adding sulfurous acid to adjust the pH value to 1.8-2.7, introducing steam, heating to 95 ℃ while stirring, and keeping for 45-60 minutes to extract most of pectin;
filtering the sleeve extraction material through a filter press, separating impurities by using a 7000 r/min high-speed centrifuge, and then rapidly cooling to about 50 ℃; adding 1-2% amylase to hydrolyze starch in the extract into sugar, heating to 77 ℃ to destroy the activity of the enzyme when the enzyme action is finished, adding 0.3-0.5% of active carbon, stirring at 55-60 ℃ for 20-30 minutes to decolorize pectin, adding 1-1.5% of diatomite, stirring uniformly, and filtering the extract by a filter press;
and step four, feeding the filtered pectin liquid into a vacuum concentration pot, keeping the vacuum degree above 667 mm Hg and the boiling point at about 50 ℃, concentrating until the total solid reaches 7-9%, after the concentration is finished, heating the pectin liquid to 70 ℃, putting the pectin liquid into a glass bottle, sealing the glass bottle with a cover, placing the glass bottle in hot water at 70 ℃, heating and sterilizing the glass bottle for 30 minutes, cooling, sealing and storing the glass bottle.
Preferably, the bacteriostatic and antiviral mechanism of the citrus flavonoid is that the chemical structure of hesperidin belongs to phenolic derivatives, and phenolic compounds and derivatives thereof are generally weakly acidic with pH of 6, can solidify or denature proteins, and thus have bacteriostatic and antiviral effects.
Preferably, the oral administration of the limonin can effectively and dose-dependently improve bleomycin-induced pulmonary fibrosis injury and inflammatory symptoms of the pathogenesis process of the mouse pulmonary fibrosis injury, and the detection of collagen synthesis shows that the limonin can down regulate the generation of alpha-SMA and collagen in a dose-dependent manner, and the effect is based on the inhibition of TGF-beta signal channels in mouse fibrotic lung tissues by phellodendron lactone.
Preferably, the pectin belongs to one of water-soluble dietary fibers, has certain viscosity, can prolong the retention time of the limonin and the citrus flavonoid in the throat to give full play to the efficacy, can form a thin protective film when reaching the stomach, can effectively relieve the stimulation of alcohol to the stomach, and simultaneously absorbs a large amount of water in the intestinal tract to keep the excrement in a wet state.
Preferably, the water-soluble fiber can effectively activate beneficial bacteria in the intestinal tract, promote mass propagation of the beneficial bacteria and create healthy ecology of the intestinal tract.
The invention has the technical effects and advantages that:
the phellodendron lactone can be applied to chronic lung diseases mediated by various inflammations including pulmonary fibrosis, chronic pneumonia, silicosis, chronic bronchitis, chronic obstructive pulmonary disease and asthma, the novel coronavirus infects serious lung inflammation injury of patients, the limonin and citrus flavonoid compounds are applied to the functional beverage, the problem that the traditional antiviral drugs have large toxic and side effects or are easy to generate drug resistance can be solved, the treatment and the later recovery of the patients are greatly facilitated, the pectin has certain viscosity, the residence time of the limonin and the citrus flavonoid in the throat can be prolonged, the effect can be fully exerted, a thin protective film can be formed when the pectin reaches the stomach, the stimulation of alcohol to the stomach can be effectively relieved, meanwhile, a large amount of water is absorbed in the intestinal tract, the feces can be kept in a wet state, and the actual effects of the limonin and the citrus flavonoid are increased, the bitter beverage has stronger efficacy of relieving the pulmonary fibrosis.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a bitter beverage for relieving pulmonary fibrosis, which comprises the following steps:
step one, taking fresh lemons, cleaning, drying, peeling, removing seeds, juicing, filtering by using 150-mesh filter cloth, removing residues, and collecting lemon juice;
adding the citrus flavone, the limonin and the pectin into the lemon juice, adding water and honey for blending, and homogenizing the blended beverage;
and step three, filling the homogenized pulp into a sterilized glass bottle, sealing the glass bottle, sterilizing the glass bottle for 15-20 min at 85-86 ℃, and finally cooling the glass bottle to room temperature to obtain the bitter beverage, wherein the bitter beverage is rich in water-soluble fibers.
The purification method of the citrus flavonoid comprises the following steps:
step one, cleaning and crushing citrus peel, putting the crushed citrus peel and 50-95 v/v% ethanol water solution in an extractor according to the weight ratio of 1: 1-5, extracting for 0.5-1 hour under the reflux state, filtering, and repeating the step for 3 times;
step two, combining the filtered filtrates, concentrating to obtain a citrus peel extract, suspending the obtained citrus peel extract in water, and performing centrifugal filtration to obtain a clear filtrate;
step three, flowing the clear filtrate through an adsorption column filled with pretreated polystyrene type adsorption resin with the granularity of 0.3-1.25 mm at the flow rate of 1.5-8 BV/h at the temperature of 20-30 ℃, wherein the diameter of the adsorption column is as follows: the height ratio is 1: 3-30;
step four, water flows through the adsorption column at the flow rate of 5-10 BV/h; and finally, flowing methanol through the adsorption column at the flow rate of 2-10 BV/h, collecting the obtained liquid, and concentrating to obtain the citrus flavonoid.
The purification method of the limonin comprises the following steps:
step one, drying and crushing sweet orange seeds, thoroughly degreasing the sweet orange seeds for 24 hours by using petroleum ether (60-90 ℃) in a Soxhlet extractor, extracting the sweet orange seeds for 6 hours by using acetone, concentrating an acetone extracting solution under reduced pressure to dryness, dissolving the acetone extracting solution by using dichloromethane and filtering;
adding isopropanol with 2 times of volume into a dichloromethane solution, uniformly mixing, placing in a refrigerator at 4 ℃, and precipitating a flaky crystal;
step three, recrystallizing the obtained crystal I for 3 times according to the solvent system for determination, evaporating the crystallized mother liquor to dryness, and performing silica gel column chromatography to 100-200 meshes, wherein the eluent is ethyl acetate: methanol 95: 5, detecting with silica gel G thin layer chromatography plate, spraying Ehrlich reagent, mixing the components with the same red spot shift value, and limonin crystal.
The pectin purifying method comprises the following steps:
step one, soaking lemon peel and squeezed pomace in clear water for half an hour, heating to 90 ℃ for 5 minutes, pressing to remove juice, and rinsing with clear water for several times, so that most of glucoside, pigment and other impurities can be removed, and most of bitter taste is removed;
step two, pouring the ground raw materials into an extraction pot, adding 4 times of water, adding sulfurous acid to adjust the pH value to 1.8-2.7, introducing steam, heating to 95 ℃ while stirring, and keeping for 45-60 minutes to extract most of pectin;
filtering the sleeve extraction material through a filter press, separating impurities by using a 7000 r/min high-speed centrifuge, and then rapidly cooling to about 50 ℃; adding 1-2% amylase to hydrolyze starch in the extract into sugar, heating to 77 ℃ to destroy the activity of the enzyme when the enzyme action is finished, adding 0.3-0.5% of active carbon, stirring at 55-60 ℃ for 20-30 minutes to decolorize pectin, adding 1-1.5% of diatomite, stirring uniformly, and filtering the extract by a filter press;
and step four, feeding the filtered pectin liquid into a vacuum concentration pot, keeping the vacuum degree above 667 mm Hg and the boiling point at about 50 ℃, concentrating until the total solid reaches 7-9%, after the concentration is finished, heating the pectin liquid to 70 ℃, putting the pectin liquid into a glass bottle, sealing the glass bottle with a cover, placing the glass bottle in hot water at 70 ℃, heating and sterilizing the glass bottle for 30 minutes, cooling, sealing and storing the glass bottle.
The antibacterial and antiviral mechanism of the citrus flavonoid is that the chemical structure of hesperidin belongs to a phenolic derivative, and the phenolic compound and the derivatives thereof are generally weakly acidic pH (6) and can solidify or denature protein, so that the hesperidin has antibacterial and antiviral effects.
The oral administration of the limonin can effectively improve bleomycin-induced pulmonary fibrosis injury of mice and inflammatory symptoms of the onset process of the pulmonary fibrosis injury of the mice in a dose-dependent manner, and detection of collagen synthesis shows that the limonin can down-regulate the generation of alpha-SMA and collagen in a dose-dependent manner, and the effect is based on the inhibition of a TGF-beta signal channel in mouse fibrosis lung tissues by phellodendron lactone.
Pectin belongs to one of water-soluble dietary fibers, has certain viscosity, can prolong the retention time of limonin and citrus flavonoid in the throat to give full play to the efficacy, can form a thin protective film when reaching the stomach, can effectively relieve the stimulation of alcohol to the stomach, and simultaneously absorbs a large amount of water in the intestinal tract to keep the feces in a wet state.
The water-soluble fiber can effectively activate beneficial bacteria in the intestinal tract, promote mass propagation of the beneficial bacteria and create healthy ecology of the intestinal tract.
The working principle of the invention is as follows: cleaning fresh fructus Citri Limoniae, drying, peeling, removing seeds, squeezing, filtering with 150 mesh filter cloth, removing residue, and collecting lemon juice; adding citrus flavone, limonin and pectin into lemon juice, adding water and honey, blending, and homogenizing the blended beverage; filling the homogenized pulp into a sterilized glass bottle, sealing the glass bottle, sterilizing the glass bottle for 15 to 20min at the temperature of between 85 and 86 ℃, and finally cooling the glass bottle to room temperature to obtain bitter beverage, wherein the bitter beverage is rich in water-soluble fibers; the phellodendron lactone can be applied to chronic lung diseases mediated by various inflammations including pulmonary fibrosis, chronic pneumonia, silicosis, chronic bronchitis, chronic obstructive pulmonary disease and asthma, the novel coronavirus infects serious lung inflammation injury of patients, the limonin and citrus flavonoid compounds are applied to the functional beverage, the problem that the traditional antiviral drugs have large toxic and side effects or are easy to generate drug resistance can be solved, the treatment and the later recovery of the patients are greatly facilitated, the pectin has certain viscosity, the residence time of the limonin and the citrus flavonoid in the throat can be prolonged, the effect can be fully exerted, a thin protective film can be formed when the pectin reaches the stomach, the stimulation of alcohol to the stomach can be effectively relieved, meanwhile, a large amount of water is absorbed in the intestinal tract, the feces can be kept in a wet state, and the actual effects of the limonin and the citrus flavonoid are increased, the bitter beverage has stronger efficacy of relieving the pulmonary fibrosis.
In the description of the present invention, unless otherwise expressly specified or limited, the terms "disposed," "mounted," "connected," and "secured" are to be construed broadly, e.g., as meaning fixedly connected, detachably connected, or integral to; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The standard parts used by the invention can be purchased from the market, and the special-shaped parts can be customized according to the description of the specification.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. A method of preparing a bitter beverage for relieving pulmonary fibrosis, comprising the steps of:
step one, taking fresh lemons, cleaning, drying, peeling, removing seeds, juicing, filtering by using 150-mesh filter cloth, removing residues, and collecting lemon juice;
adding the citrus flavone, the limonin and the pectin into the lemon juice, adding water and honey for blending, and homogenizing the blended beverage;
and step three, filling the homogenized pulp into a sterilized glass bottle, sealing the glass bottle, sterilizing the glass bottle for 15-20 min at 85-86 ℃, and finally cooling the glass bottle to room temperature to obtain the bitter beverage, wherein the bitter beverage is rich in water-soluble fibers.
2. The method of preparing a bitter beverage for relieving pulmonary fibrosis as recited in claim 1 wherein the purifying process of citrus flavonoid comprises the steps of:
step one, cleaning and crushing citrus peel, putting the crushed citrus peel and 50-95 v/v% ethanol water solution in an extractor according to the weight ratio of 1: 1-5, extracting for 0.5-1 hour under the reflux state, filtering, and repeating the step for 3 times;
step two, combining the filtered filtrates, concentrating to obtain a citrus peel extract, suspending the obtained citrus peel extract in water, and performing centrifugal filtration to obtain a clear filtrate;
step three, flowing the clear filtrate through an adsorption column filled with pretreated polystyrene type adsorption resin with the granularity of 0.3-1.25 mm at the flow rate of 1.5-8 BV/h at the temperature of 20-30 ℃, wherein the diameter of the adsorption column is as follows: the height ratio is 1: 3-30;
step four, water flows through the adsorption column at the flow rate of 5-10 BV/h; and finally, flowing methanol through the adsorption column at the flow rate of 2-10 BV/h, collecting the obtained liquid, and concentrating to obtain the citrus flavonoid.
3. The method of claim 1, wherein the purification of limonin comprises the steps of:
step one, drying and crushing sweet orange seeds, thoroughly degreasing the sweet orange seeds for 24 hours by using petroleum ether (60-90 ℃) in a Soxhlet extractor, extracting the sweet orange seeds for 6 hours by using acetone, concentrating an acetone extracting solution under reduced pressure to dryness, dissolving the acetone extracting solution by using dichloromethane and filtering;
adding isopropanol with 2 times of volume into a dichloromethane solution, uniformly mixing, placing in a refrigerator at 4 ℃, and precipitating a flaky crystal;
step three, recrystallizing the obtained crystal I for 3 times according to the solvent system for determination, evaporating the crystallized mother liquor to dryness, and performing silica gel column chromatography to 100-200 meshes, wherein the eluent is ethyl acetate: methanol 95: 5, detecting with silica gel G thin layer chromatography plate, spraying Ehrlich reagent, mixing the components with the same red spot shift value, and limonin crystal.
4. The method of claim 1, wherein the pectin purification process comprises the steps of:
step one, soaking lemon peel and squeezed pomace in clear water for half an hour, heating to 90 ℃ for 5 minutes, pressing to remove juice, and rinsing with clear water for several times, so that most of glucoside, pigment and other impurities can be removed, and most of bitter taste is removed;
step two, pouring the ground raw materials into an extraction pot, adding 4 times of water, adding sulfurous acid to adjust the pH value to 1.8-2.7, introducing steam, heating to 95 ℃ while stirring, and keeping for 45-60 minutes to extract most of pectin;
filtering the sleeve extraction material through a filter press, separating impurities by using a 7000 r/min high-speed centrifuge, and then rapidly cooling to about 50 ℃; adding 1-2% amylase to hydrolyze starch in the extract into sugar, heating to 77 ℃ to destroy the activity of the enzyme when the enzyme action is finished, adding 0.3-0.5% of active carbon, stirring at 55-60 ℃ for 20-30 minutes to decolorize pectin, adding 1-1.5% of diatomite, stirring uniformly, and filtering the extract by a filter press;
and step four, feeding the filtered pectin liquid into a vacuum concentration pot, keeping the vacuum degree above 667 mm Hg and the boiling point at about 50 ℃, concentrating until the total solid reaches 7-9%, after the concentration is finished, heating the pectin liquid to 70 ℃, putting the pectin liquid into a glass bottle, sealing the glass bottle with a cover, placing the glass bottle in hot water at 70 ℃, heating and sterilizing the glass bottle for 30 minutes, cooling, sealing and storing the glass bottle.
5. The method of claim 1, wherein the anti-bacterial and antiviral mechanism of citrus flavonoid is that hesperidin has a chemical structure of phenolic derivatives, phenolic compounds and derivatives thereof, generally having a weak acidic PH of 6, and is capable of coagulating or denaturing proteins, thereby having anti-bacterial and antiviral effects.
6. The method of claim 1, wherein the oral administration of limonin is effective to dose-dependently ameliorate the inflammatory symptoms of bleomycin-induced pulmonary fibrosis injury and its pathogenesis in mice, and the detection of collagen synthesis indicates that limonin can dose-dependently down-regulate the production of α -SMA and collagen, based on the inhibition of TGF- β signaling pathway in fibrotic lung tissue in mice by phellodendron lactone.
7. The method of claim 1, wherein the pectin is one of water-soluble dietary fibers, has viscosity, and is effective in prolonging the residence time of limonin and citrus flavonoid in the throat to form a thin protective film on the stomach, thereby effectively relieving the irritation of alcohol to the stomach, and absorbing a large amount of water in the intestinal tract to keep the feces in a wet state.
8. The method of claim 1, wherein the water-soluble fiber is effective to activate beneficial bacteria in the intestinal tract, promote mass propagation of beneficial bacteria, and create a healthy gut ecology.
CN202111439198.XA 2021-11-30 2021-11-30 Preparation method of bitter beverage for relieving pulmonary fibrosis Pending CN114097965A (en)

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