CN114794159A - Composition containing camellia saponin as main component for preventing and treating Chinese rose diseases and preparation method thereof - Google Patents

Composition containing camellia saponin as main component for preventing and treating Chinese rose diseases and preparation method thereof Download PDF

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CN114794159A
CN114794159A CN202210627157.1A CN202210627157A CN114794159A CN 114794159 A CN114794159 A CN 114794159A CN 202210627157 A CN202210627157 A CN 202210627157A CN 114794159 A CN114794159 A CN 114794159A
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anthraquinone
orange peel
main component
camellia
preventing
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涂佳
李昌珠
肖志红
李党训
李力
吉悦娜
肖静晶
刘思思
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Hunan Academy of Forestry
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Hunan Academy of Forestry
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N35/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
    • A01N35/06Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing keto or thioketo groups as part of a ring, e.g. cyclohexanone, quinone; Derivatives thereof, e.g. ketals
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/42Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing within the same carbon skeleton a carboxylic group or a thio analogue, or a derivative thereof, and a carbon atom having only two bonds to hetero atoms with at the most one bond to halogen, e.g. keto-carboxylic acids
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/14Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
    • A01N65/30Polygonaceae [Buckwheat family], e.g. red-knees or rhubarb
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
    • A01N65/36Rutaceae [Rue family], e.g. lime, orange, lemon, corktree or pricklyash

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Abstract

The invention discloses a composition taking camellia saponin as a main component for preventing and treating Chinese rose diseases and a preparation method thereof, relating to the technical field of disease-preventing compositions, wherein the composition taking camellia saponin as the main component for preventing and treating Chinese rose diseases comprises the following components: 5-8 parts of camellia saponin, 1-2.5 parts of orange peel flavone and 1-2.5 parts of anthraquinone bacteriostatic agent by mass; the preparation method comprises the following steps: firstly, preparing sasanquasaponin: secondly, preparing orange peel flavone: thirdly, preparing anthraquinone bacteriostat: fourthly, mixing the sasanquasaponin, the orange peel flavone and the anthraquinone bacteriostatic agent; fifthly, adjusting the pH value of the mixed solution; the composition which takes the camellia saponin as the main component and is used for preventing and treating the diseases of the Chinese roses is prepared by using the camellia saponin, the tangerine peel flavone and the anthraquinone bacteriostatic agent, has obvious effect on inhibiting the diseases of the Chinese roses, effectively prevents the phenomenon of yellow leaves falling caused by plum rain season, promotes the bud germination of the Chinese roses and ensures that the Chinese roses are luxuriant with leaves.

Description

Composition containing camellia saponin as main component for preventing and treating Chinese rose diseases and preparation method thereof
Technical Field
The invention relates to the technical field of disease-preventing compositions, in particular to a composition which takes camellia saponin as a main component and is used for preventing and treating diseases of China roses and a preparation method thereof.
Background
In modern agricultural production, a method for preventing and treating plant diseases mainly adopts spraying of chemical pesticides, traditional pesticides are easy to decompose when exposed to light and run off along with rain wash, and once the pesticides run off, the pesticide application effect of plants is affected and soil is polluted; black spot and powdery mildew in diseases of Chinese roses are common, and the influence on the Chinese roses is large; therefore, the black spot and the powdery mildew are the key points for preventing and controlling the diseases of the Chinese rose; yellow leaves and fallen leaves appear in plum rain seasons, so that a natural product is found to replace a composition of chemical pesticides, and the composition is adopted to inhibit diseases of Chinese roses and promote the growth of the Chinese roses to become important points of attention of people; therefore, in view of the current situation, there is an urgent need to develop a composition containing sasanquasaponin as a main component for preventing and treating rosa chinensis diseases and a preparation method thereof, so as to meet the needs of practical use.
Disclosure of Invention
In view of the above, the present invention provides a composition containing sasanquasaponin as a main component for preventing and treating a disease of rosa chinensis and a preparation method thereof, wherein sasanquasaponin, tangeretin and anthraquinone bacteriostatic agents are used to prepare the composition containing sasanquasaponin as a main component for preventing and treating the disease of rosa chinensis.
In order to achieve the purpose, the invention adopts the following technical scheme:
a composition taking sasanquasaponin as a main component for preventing and treating Chinese rose diseases comprises the following components: the bacteriostatic agent comprises 5-8 parts by mass of camellia saponin, 1-2.5 parts by mass of orange peel flavone and 1-2.5 parts by mass of anthraquinone bacteriostatic agent; the anthraquinone bacteriostatic agent comprises rhein, aloe-emodin, chrysophanol glucoside, emodin glucoside, physcion glucoside and chrysophanol.
As a preferred embodiment: the oil tea saponin, the tangerine peel flavone and the anthraquinone bacteriostatic agent are mixed according to the mass part ratio of 8:1: 1; the anthraquinone bacteriostatic agent comprises the following components in percentage by weight: rhein 20-30 wt%, aloe-emodin 10-15 wt%, emodin 15-20 wt%, chrysophanol glucoside 12-18 wt%, emodin glucoside 16-20 wt%, physcion glucoside 5-8 wt% and chrysophanol 13-15 wt%.
The preparation method of the composition taking the camellia saponin as the main component for preventing and treating the diseases of the Chinese roses comprises the following steps:
firstly, preparing sasanquasaponin: crushing raw material camellia oleifera, adding purified water into the crushed raw material camellia oleifera, performing heating reflux extraction for 2.5 to 3.5 hours at the temperature of 95 to 100 ℃, filtering to obtain camellia saponin extraction filtrate, and concentrating the camellia saponin extraction filtrate until the solid content is 10 to 20 percent to obtain camellia saponin concentrated solution;
secondly, preparing orange peel flavone: crushing orange peel, and performing ultrasonic extraction, filtration and reduced pressure concentration on the crushed orange peel powder to obtain an orange peel flavone crude extract; purifying the crude extract of the orange peel flavone by adopting a polyamide resin column, eluting by adopting 40-80% ethanol as an eluent, wherein the volume ratio of the mass of orange peel to the volume of the ethanol is 1: 10-1: 60g/mL, and obtaining an orange peel flavone extract;
thirdly, preparing anthraquinone bacteriostat: pulverizing radix et rhizoma Rhei into coarse powder, extracting with water under reflux, filtering, and mixing filtrates; concentrating the combined filtrate under reduced pressure to obtain water extract concentrated solution, and adding 30% -80% ethanol, heating and reflux extracting to obtain chrysophanol concentrated solution; separating and purifying the chrysophanol concentrated solution by adopting macroporous adsorption resin to obtain anthraquinone bacteriostats of each component;
fourthly, preparation of the composition: dissolving the camellia saponin concentrated solution, the orange peel flavone extract and the anthraquinone bacteriostatic agent in water, stirring and uniformly mixing to obtain a mixed solution, and concentrating the mixed solution under reduced pressure to obtain a composition concentrated solution;
and fifthly, adjusting the pH value of the mixed solution to be 5-6, and then carrying out ultrasonic treatment or stirring to obtain the composition which is used for preventing and treating the diseases of the Chinese roses and takes the sasanquasaponin as a main component.
As a preferred embodiment: in the first step, the raw material oil tea is crushed into 10-30 meshes, and purified water is added into the crushed raw material oil tea, wherein the mass of the purified water is 7-9 times that of the raw material oil tea; the temperature at which the extraction was carried out under heating and refluxing was 98 ℃.
As a preferred embodiment: the ultrasonic extraction process in the step two comprises the following steps: the ultrasonic power is 500-600W, and the ultrasonic extraction temperature is 60-70 ℃.
As a preferred embodiment: the conditions of reduced pressure concentration in the second step are as follows: under the vacuum of-0.2 MPa, the rotating speed is 110-1150 rpm/min, and the evaporation temperature is 45-48 ℃.
As a preferred embodiment: in the second step, the polyamide resin column is filled with 65-70% ethanol as eluent.
As a preferred embodiment: in the third step, macroporous adsorption resin is adopted to separate and purify the chrysophanol concentrated solution, and the eluent is 30-95% ethanol.
As a preferred embodiment: in the fourth step, the concentrated solution of the oil tea saponin, the orange peel flavone extract and the anthraquinone bacteriostat are dissolved in water and heated for 30min at 70-80 ℃ to obtain a mixed solution.
As a preferred embodiment: and in the fifth step, the pH value is adjusted by using citric acid-sodium bicarbonate, and the pH value is 6.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and concretely, according to the technical scheme, the composition which takes the camellia saponin as the main component and is used for preventing and treating the diseases of the Chinese roses is prepared by using the camellia saponin, the tangerine peel flavone and the anthraquinone bacteriostat, the composition has obvious effect on inhibiting the diseases of the Chinese roses, can effectively prevent yellow leaves from falling off caused by the fungus in the plum rain season, promotes the germination of the buds of the Chinese roses and has luxuriant branches and leaves; in the prior art, toxic pesticides or antibiotics are mostly adopted to prevent and treat the diseases of the Chinese roses, and natural products are used for replacing chemical pesticides, so that the disease prevention effect is good.
Detailed Description
To more clearly illustrate the structural features and effects of the present invention, the following detailed description is given with reference to specific examples.
Example 1
The composition taking the camellia saponin as a main component for preventing and treating the diseases of the Chinese roses comprises the following components: the bacteriostatic agent comprises 5 parts by mass of camellia saponin, 2.5 parts by mass of orange peel flavone and 2.5 parts by mass of anthraquinone bacteriostatic agent; the anthraquinone bacteriostatic agent comprises rhein, aloe-emodin, chrysophanol glucoside, emodin glucoside, physcion glucoside and chrysophanol.
The preparation method of the composition taking the camellia saponin as the main component for preventing and treating the diseases of the Chinese roses comprises the following steps:
firstly, preparing sasanquasaponin: crushing raw material tea into 10 meshes, adding purified water with the mass being 7 times of that of the raw material camellia oleifera into the crushed raw material tea, heating and refluxing for extraction for 2.5 hours at the temperature of 98 ℃, filtering to obtain camellia saponin extraction filtrate, and concentrating the camellia saponin extraction filtrate until the solid content is 10% to obtain camellia saponin concentrated solution;
secondly, preparing the orange peel flavone: crushing orange peel, and performing ultrasonic extraction, filtration and reduced pressure concentration on the crushed orange peel powder to obtain an orange peel flavone crude extract; the ultrasonic power is 500W, and the ultrasonic extraction temperature is 60 ℃; the conditions for concentration under reduced pressure were: under the vacuum of-0.2 MPa, the rotating speed is 110rpm/min, and the evaporation temperature is 45 ℃; purifying the crude extract of the orange peel flavone by adopting a polyamide resin column, and eluting by adopting ethanol with the concentration of 70% as eluent, wherein the volume ratio of the orange peel mass to the ethanol is 1:10g/mL to obtain an orange peel flavone extract;
thirdly, preparing anthraquinone bacteriostat: pulverizing radix et rhizoma Rhei into coarse powder, extracting with water under reflux, filtering, and mixing filtrates; concentrating the combined filtrate under reduced pressure to obtain water extract concentrated solution, adding 80% ethanol, heating and reflux extracting to obtain chrysophanol concentrated solution; separating and purifying the chrysophanol concentrated solution by adopting macroporous adsorption resin, wherein the eluent is 95% ethanol to obtain anthraquinone bacteriostats of each component;
fourthly, preparation of the composition: dissolving the concentrated solution of sasanquasaponin, the extract of orange peel flavone and anthraquinone bacteriostatic agent in water, heating at 80 deg.C for 30min, stirring to obtain mixed solution, and concentrating the mixed solution under reduced pressure to obtain concentrated solution of composition; wherein the mass ratio of the sasanquasaponin to the tangerine peel flavone to the anthraquinone bacteriostatic agent is 5:2.5: 2.5;
and fifthly, adjusting the pH value of the mixed solution, adjusting the pH value to be 6 by using citric acid-sodium bicarbonate, and then performing ultrasonic treatment or stirring to obtain the composition which is used for preventing and treating the diseases of the Chinese roses and takes the sasanquasaponin as a main component.
Example 2
The composition taking the camellia saponin as a main component for preventing and treating the diseases of the Chinese roses comprises the following components: the bacteriostatic agent comprises camellia saponin, tangerine peel flavone and anthraquinone bacteriostatic agent, wherein the components comprise 6 parts of camellia saponin, 2 parts of tangerine peel flavone and 2 parts of anthraquinone bacteriostatic agent by mass; the anthraquinone bacteriostatic agent comprises rhein, aloe-emodin, chrysophanol glucoside, emodin glucoside, physcion glucoside and chrysophanol.
The preparation method of the composition taking the camellia saponin as the main component for preventing and treating the diseases of the Chinese roses comprises the following steps:
firstly, preparing sasanquasaponin: crushing raw material tea into 10 meshes, adding purified water which is 9 times of the weight of the raw material camellia into the crushed raw material tea, heating and refluxing for extraction for 2.5 hours at the temperature of 98 ℃, filtering to obtain camellia saponin extraction filtrate, and concentrating the camellia saponin extraction filtrate until the solid content is 10% to obtain camellia saponin concentrated solution;
secondly, preparing orange peel flavone: crushing orange peel, and performing ultrasonic extraction, filtration and reduced pressure concentration on the crushed orange peel powder to obtain an orange peel flavone crude extract; the ultrasonic power is 500W, and the ultrasonic extraction temperature is 60 ℃; the conditions for concentration under reduced pressure were: under the vacuum of-0.2 MPa, the rotating speed is 110rpm/min, and the evaporation temperature is 45 ℃; purifying the crude extract of the orange peel flavone by adopting a polyamide resin column, and eluting by adopting 65% ethanol as an eluent, wherein the volume ratio of the orange peel mass to the ethanol is 1:10g/mL to obtain an orange peel flavone extract;
thirdly, preparing anthraquinone bacteriostat: pulverizing radix et rhizoma Rhei into coarse powder, extracting with water under reflux, filtering, and mixing filtrates; concentrating the combined filtrate under reduced pressure to obtain water extract concentrated solution, adding 80% ethanol, heating and reflux extracting to obtain chrysophanol concentrated solution; separating and purifying the chrysophanol concentrated solution by adopting macroporous adsorption resin, wherein the eluent is 95% ethanol to obtain anthraquinone bacteriostats of each component;
fourthly, preparation of the composition: dissolving the concentrated solution of sasanquasaponin, the extract of orange peel flavone and anthraquinone bacteriostatic agent in water, heating at 80 deg.C for 30min, stirring to obtain mixed solution, and concentrating the mixed solution under reduced pressure to obtain concentrated solution of composition; wherein the mass ratio of the sasanquasaponin to the tangerine peel flavone to the anthraquinone bacteriostatic agent is 6:2: 2;
and fifthly, adjusting the pH value of the mixed solution, adjusting the pH value to be 6 by using citric acid-sodium bicarbonate, and then performing ultrasonic treatment or stirring to obtain the composition which is used for preventing and treating the diseases of the Chinese roses and takes the camellia saponin as the main component.
Example 3
The composition taking the camellia saponin as a main component for preventing and treating the diseases of the Chinese roses comprises the following components: the bacteriostatic agent comprises, by mass, 7 parts of camellia saponin, 1.5 parts of orange peel flavone and 1.5 parts of anthraquinone bacteriostatic agent; the anthraquinone bacteriostatic agent comprises rhein, aloe-emodin, chrysophanol glucoside, emodin glucoside, physcion glucoside and chrysophanol.
The preparation method of the composition taking the camellia saponin as the main component for preventing and treating the diseases of the Chinese roses comprises the following steps:
firstly, preparing sasanquasaponin: crushing raw material tea into 30 meshes, adding purified water with the mass being 9 times of that of the raw material camellia into the crushed raw material tea, performing heating reflux extraction at the temperature of 98 ℃ for 2.5 hours, filtering to obtain camellia saponin extraction filtrate, and concentrating the camellia saponin extraction filtrate until the solid content is 10% to obtain camellia saponin concentrated solution;
secondly, preparing orange peel flavone: crushing orange peel, and performing ultrasonic extraction, filtration and reduced pressure concentration on the crushed orange peel powder to obtain an orange peel flavone crude extract; the ultrasonic power is 500W, and the ultrasonic extraction temperature is 60 ℃; the conditions for concentration under reduced pressure were: under the vacuum of-0.2 MPa, the rotating speed is 110rpm/min, and the evaporation temperature is 45 ℃; purifying the crude extract of the orange peel flavone by adopting a polyamide resin column, and eluting by adopting 65% ethanol as an eluent, wherein the volume ratio of the orange peel mass to the ethanol is 1:60g/mL to obtain an orange peel flavone extract;
thirdly, preparing anthraquinone bacteriostat: pulverizing radix et rhizoma Rhei into coarse powder, extracting with water under reflux, filtering, and mixing filtrates; concentrating the combined filtrate under reduced pressure to obtain water extract concentrated solution, adding 80% ethanol, heating and reflux extracting to obtain chrysophanol concentrated solution; separating and purifying the chrysophanol concentrated solution by adopting macroporous adsorption resin, wherein the eluent is 95% ethanol to obtain anthraquinone bacteriostats of each component;
fourthly, preparation of the composition: dissolving the concentrated solution of sasanquasaponin, the extract of orange peel flavone and anthraquinone bacteriostatic agent in water, heating at 80 deg.C for 30min, stirring to obtain mixed solution, and concentrating the mixed solution under reduced pressure to obtain concentrated solution of composition; wherein the mass ratio of the sasanquasaponin to the tangerine peel flavone to the anthraquinone bacteriostatic agent is 7:1.5: 1.5;
and fifthly, adjusting the pH value of the mixed solution, adjusting the pH value to be 6 by using citric acid-sodium bicarbonate, and then performing ultrasonic treatment or stirring to obtain the composition which is used for preventing and treating the diseases of the Chinese roses and takes the sasanquasaponin as a main component.
Example 4
The composition taking the camellia saponin as a main component for preventing and treating the diseases of the Chinese roses comprises the following components: the bacteriostatic agent comprises 8 parts by mass of camellia saponin, 1 part by mass of orange peel flavone and 1 part by mass of anthraquinone bacteriostatic agent; the anthraquinone bacteriostatic agent comprises rhein, aloe-emodin, chrysophanol glucoside, emodin glucoside, physcion glucoside and chrysophanol.
The preparation method of the composition taking the camellia saponin as the main component for preventing and treating the diseases of the Chinese roses comprises the following steps:
firstly, preparing sasanquasaponin: crushing raw material tea into 30 meshes, adding purified water with the mass being 9 times of that of the raw material camellia into the crushed raw material tea, performing heating reflux extraction at the temperature of 98 ℃ for 2.5 hours, filtering to obtain camellia saponin extraction filtrate, and concentrating the camellia saponin extraction filtrate until the solid content is 10% to obtain camellia saponin concentrated solution;
secondly, preparing orange peel flavone: crushing orange peel, and performing ultrasonic extraction, filtration and reduced pressure concentration on the crushed orange peel powder to obtain an orange peel flavone crude extract; the ultrasonic power is 500W, and the ultrasonic extraction temperature is 60 ℃; the conditions for concentration under reduced pressure were: under the vacuum of-0.2 MPa, the rotating speed is 110rpm/min, and the evaporation temperature is 45 ℃; purifying the crude extract of the orange peel flavone by adopting a polyamide resin column, and eluting by adopting 65% ethanol as an eluent, wherein the volume ratio of the orange peel mass to the ethanol is 1:60g/mL to obtain an orange peel flavone extract;
thirdly, preparing anthraquinone bacteriostat: pulverizing radix et rhizoma Rhei into coarse powder, extracting with water under reflux, filtering, and mixing filtrates; concentrating the combined filtrate under reduced pressure to obtain water extract concentrated solution, adding 80% ethanol, heating and reflux extracting to obtain chrysophanol concentrated solution; separating and purifying the chrysophanol concentrated solution by adopting macroporous adsorption resin, wherein the eluent is 95% ethanol to obtain anthraquinone bacteriostats of each component;
fourthly, preparation of the composition: dissolving the concentrated solution of sasanquasaponin, the extract of orange peel flavone and anthraquinone bacteriostatic agent in water, heating at 80 deg.C for 30min, stirring to obtain mixed solution, and concentrating the mixed solution under reduced pressure to obtain concentrated solution of composition; wherein the mass ratio of the sasanquasaponin to the tangerine peel flavone to the anthraquinone bacteriostatic agent is 8:1: 1;
and fifthly, adjusting the pH value of the mixed solution, adjusting the pH value to be 6 by using citric acid-sodium bicarbonate, and then performing ultrasonic treatment or stirring to obtain the composition which is used for preventing and treating the diseases of the Chinese roses and takes the sasanquasaponin as a main component.
Comparative example 1
Compared with example 1, the difference is only that no sasanquasaponin is contained.
A composition for controlling rose diseases, comprising the following components: orange peel flavone and anthraquinone bacteriostatic agent, wherein each component is calculated according to the part by mass and 2.5 parts of orange peel flavone and 2.5 parts of anthraquinone bacteriostatic agent; the anthraquinone bacteriostatic agent comprises rhein, aloe-emodin, chrysophanol glucoside, emodin glucoside, physcion glucoside and chrysophanol.
The preparation method of the composition for preventing and treating the diseases of the Chinese roses comprises the following steps:
firstly, preparing orange peel flavone: crushing orange peel, and performing ultrasonic extraction, filtration and reduced pressure concentration on the crushed orange peel powder to obtain an orange peel flavone crude extract; the ultrasonic power is 500W, and the ultrasonic extraction temperature is 60 ℃; the conditions for concentration under reduced pressure were: under the vacuum of-0.2 MPa, the rotating speed is 110rpm/min, and the evaporation temperature is 45 ℃; purifying the crude extract of the orange peel flavone by adopting a polyamide resin column, eluting by adopting 70% ethanol as eluent, wherein the volume ratio of the mass of the orange peel to the ethanol is 1:10g/mL, and obtaining an orange peel flavone extract;
secondly, preparing anthraquinone bacteriostat: pulverizing radix et rhizoma Rhei into coarse powder, extracting with water under reflux, filtering, and mixing filtrates; concentrating the combined filtrate under reduced pressure to obtain water extract concentrated solution, adding 80% ethanol, heating and reflux extracting to obtain chrysophanol concentrated solution; separating and purifying the chrysophanol concentrated solution by adopting macroporous adsorption resin, wherein the eluent is 95% ethanol to obtain anthraquinone bacteriostats of each component;
thirdly, preparing the composition: dissolving orange peel flavone extract and anthraquinone bacteriostatic agent in water, heating at 80 deg.C for 30min, stirring to obtain mixed solution, and concentrating under reduced pressure to obtain composition concentrated solution; wherein the mass ratio of the orange peel flavone to the anthraquinone bacteriostatic agent is 1: 1;
fourthly, adjusting the pH value of the mixed solution, adjusting the pH value to be equal to 6 by using citric acid-sodium bicarbonate, and then carrying out ultrasonic treatment or stirring to obtain the composition.
Comparative example 2
Compared with example 1, the difference is that no orange peel flavone is contained.
A composition for controlling rose diseases, comprising the following components: the bacteriostatic agent comprises 5 parts of camellia saponin and 2.5 parts of anthraquinone bacteriostatic agent by mass; the anthraquinone bacteriostatic agent comprises rhein, aloe-emodin, chrysophanol glucoside, emodin glucoside, physcion glucoside and chrysophanol.
The preparation method of the composition for preventing and treating the diseases of the Chinese roses comprises the following steps:
firstly, preparing sasanquasaponin: crushing raw material tea into 10 meshes, adding purified water with the mass being 7 times of that of the raw material camellia oleifera into the crushed raw material tea, heating and refluxing for extraction for 2.5 hours at the temperature of 98 ℃, filtering to obtain camellia saponin extraction filtrate, and concentrating the camellia saponin extraction filtrate until the solid content is 10% to obtain camellia saponin concentrated solution;
secondly, preparing anthraquinone bacteriostat: pulverizing radix et rhizoma Rhei into coarse powder, extracting with water under reflux, filtering, and mixing filtrates; concentrating the combined filtrate under reduced pressure to obtain water extract concentrated solution, adding 80% ethanol, heating and reflux extracting to obtain chrysophanol concentrated solution; separating and purifying the chrysophanol concentrated solution by adopting macroporous adsorption resin, wherein the eluent is 95% ethanol to obtain anthraquinone bacteriostats of each component;
thirdly, preparing the composition: dissolving the camellia saponin concentrated solution and the anthraquinone bacteriostatic agent in water, heating at 80 ℃ for 30min, stirring and uniformly mixing to obtain a mixed solution, and concentrating the mixed solution under reduced pressure to obtain a composition concentrated solution; wherein the mass ratio of the sasanquasaponin to the anthraquinone bacteriostatic agent is 2: 1;
fourthly, adjusting the pH value of the mixed solution, adjusting the pH value to be equal to 6 by using citric acid-sodium bicarbonate, and then carrying out ultrasonic treatment or stirring to obtain the composition.
Comparative example 3
Compared with example 1, the difference is that no anthraquinone bacteriostat is contained.
A composition for controlling rose diseases, comprising the following components: the tea-oil tree saponin and the orange peel flavone, wherein each component comprises 5 parts of tea-oil tree saponin and 2.5 parts of orange peel flavone by mass;
the preparation method of the composition for preventing and treating the diseases of the Chinese roses comprises the following steps:
firstly, preparing sasanquasaponin: crushing raw material tea into 10 meshes, adding purified water with the mass being 7 times of that of the raw material camellia into the crushed raw material tea, performing heating reflux extraction at the temperature of 98 ℃ for 2.5 hours, filtering to obtain camellia saponin extraction filtrate, and concentrating the camellia saponin extraction filtrate until the solid content is 10% to obtain camellia saponin concentrated solution;
secondly, preparing orange peel flavone: crushing orange peel, and performing ultrasonic extraction, filtration and reduced pressure concentration on the crushed orange peel powder to obtain an orange peel flavone crude extract; the ultrasonic power is 500W, and the ultrasonic extraction temperature is 60 ℃; the conditions for concentration under reduced pressure were: under the vacuum of-0.2 MPa, the rotating speed is 110rpm/min, and the evaporation temperature is 45 ℃; purifying the crude extract of the orange peel flavone by adopting a polyamide resin column, and eluting by adopting ethanol with the concentration of 70% as eluent, wherein the volume ratio of the orange peel mass to the ethanol is 1:10g/mL to obtain an orange peel flavone extract;
dissolving the camellia saponin concentrated solution and the orange peel flavone extract in water, heating at 80 ℃ for 30min, stirring and uniformly mixing to obtain a mixed solution, and concentrating the mixed solution under reduced pressure to obtain a composition concentrated solution; wherein the mass ratio of the sasanquasaponin to the orange peel flavone is 2: 1;
fourthly, adjusting the pH value of the mixed solution, adjusting the pH value to be equal to 6 by using citric acid-sodium bicarbonate, and then carrying out ultrasonic treatment or stirring to obtain the composition.
Effect example 1
Black spot is one of the most common and classical diseases of Chinese roses, the pathogen of which is roselle calystegia, and the disease is represented by black spots on leaves; powdery mildew is the second classic disease of China rose, the pathogen of the powdery mildew is Rosa monococcus, the occurrence frequency is next to that of black spots, the powdery mildew begins to occur at new branches and tender tips (including buds), and when the new branches are serious, the tender branches of the new branches are blackened and necrotized, and even the whole plant is died of; common diseases of Chinese roses also include gray mold: the pathogen is Botrytis cinerea; downy mildew disease: the pathogen is downy mildew; rust disease: the pathogen is rust of Rosa polyspora; branch blight: the pathogeny is mainly coniothyrium minitans; root cancer: the pathogen is bacteria of genus Yellobacterium; mosaic disease: the pathogen is China rose mosaic virus; the sasanquasaponin and the orange peel flavone have good antibacterial and antivirus effects; the anthraquinone bacteriostatic agent has broad-spectrum disease control capability and has good inhibition effect on ten fungal and bacterial diseases, such as gray mold, downy mildew, rust disease, branch blight, root cancer and mosaic disease; the composition which is prepared by the application and used for preventing and treating the diseases of the Chinese roses and takes the sasanquasaponin as the main component has the effects of preventing leaf yellowing and leaf falling caused by fungus in plum rain, promoting plant growth, promoting flower bud germination and promoting Chinese rose multiplication and leafiness; the composition for preventing and treating the diseases of the Chinese roses, which is prepared by the application and takes the sasanquasaponin as the main component, not only has bacteriostatic activity, but also induces the accumulation of phytoalexin and phenolic compounds in plants and induces the plants to generate disease resistance against pathogens.
The method comprises the steps of respectively spraying the same amount of the composition which is prepared in the embodiments 1-4 and is used for preventing and treating the Chinese rose diseases and takes the camellia saponin as a main component and the same amount of the compositions prepared in the comparative examples 1-3 to seven groups of Chinese rose leaves, wherein the other group is a blank control test and the compositions are not sprayed; the eight groups of Chinese roses have the same growth period, each group of Chinese roses is 100, and the composition is sprayed once every seven days and is continuously applied for three times; observing the change of the Chinese rose, and counting the occurrence degree of the Chinese rose diseases after the application of the compositions of the examples and the comparative examples after the observation period is ended; the number of diseased plants and the incidence of disease for each example and comparative example are shown in Table 1;
the formula for calculating the incidence is as follows:
incidence rate (number of diseased plants/number of investigated plants) × 100
Table 1: number of diseased plants and incidence of diseases of Chinese rose samples
Figure BDA0003678213150000121
As can be seen from Table 1, the incidence rates of black spot and gray spot of the Chinese rose plants treated by the compositions prepared in examples 1 to 4 are greatly reduced, and the disease index is correspondingly lower; with the increase of the mass proportion of the sasanquasaponin, the number of Chinese rose diseased plants is reduced, which indicates that the sasanquasaponin plays a main role in disease control in the prepared composition.
Effect example 2
Activity inhibition test for pathogenic bacteria of melasma and powdery mildew
The pathogen of the black spot is Erysipelothrix roseum; the pathogen of powdery mildew is Rosa monocytogenes; the tests were carried out in sixteen groups, eight of which correspond to the tests of example 1 to example 4, comparative example 1 to comparative example 3 and the control group for inhibiting Erwinia roseosporus which is black spot; eight additional tests corresponding to example 1-example 4, comparative example 1-comparative example 3 and the control group for inhibiting Erysiphe rosea of northern leaf blight; the test method comprises the following steps: the method is carried out by adopting a mycelium growth rate inhibition method according to the agricultural industry standard NY/Y156.22006 of the people's republic of China: firstly, adding the compositions prepared in examples 1-4, the compositions prepared in comparative examples 1-3 and a control group (clear water) into a culture medium, shaking up, pouring the culture medium into a culture dish with the diameter of 6cm in equal quantity, and preparing a sample-containing flat plate with corresponding concentration; after the culture medium is cooled and solidified, a sterilization puncher with the diameter of 5mm is used for punching a bacterial cake on the same circumference close to the edge of a bacterial colony, the bacterial cake is inoculated to the center of the culture medium containing a sample, the hypha surface faces downwards, a dish cover is covered, and the culture medium is placed in a constant temperature incubator at the temperature of 30 ℃ for culture, wherein the humidity is 60%; when the colonies of the control culture dish are close to the edge of the culture dish, measuring the diameter of each treated colony by using a caliper, wherein the unit is mm; vertically measuring the diameter of each culture dish by a cross method for each time, and taking an average value; the hyphal growth inhibition rate was calculated according to the following formula.
Hypha inhibition (%) - (control colony growth diameter-treated colony growth diameter)/control colony growth diameter 100
Table 2: examples 1-4, comparative examples 1-3 and control group for the inhibition of Erysiphe rosea and Erysiphe rosae of powdery mildew of northern blotch
Figure BDA0003678213150000131
The results in table 2 show that the compositions prepared in examples 1 to 4 and containing sasanquasaponin as a main component for preventing and treating rosa chinensis diseases have higher inhibitory activity against erwinia rosea sporulata of rosa chinensis and rosa multiflora of powdery mildew, and the inhibitory effect on rosa chinensis disease bacteria is better with the increase of the mass ratio of sasanquasaponin in examples 1 to 4; when the mass ratio of the sasanquasaponin to the tangerine peel flavone to the anthraquinone bacteriostatic agent is 8:1:1, the inhibition effect on Erysipelis rosea of black spot and Erysipelis rosea of powdery mildew is optimal; the comparative examples 1 to 3 show that the bacteriostatic effect is poor when no camellia saponin is added, which indicates that camellia saponin plays a main role in inhibiting pathogenic bacteria in the prepared composition.
Effect example 3
Resistance to yellow leaf cast by fungus in plum rain season:
respectively spraying the same amount of the composition which is prepared in the examples 1-4 and is used for preventing and treating the diseases of the Chinese roses and takes the sasanquaside as the main component and the compositions prepared in the comparative examples 1-3 to seven groups of Chinese rose leaves, wherein the other group is a blank control test and is not sprayed with the compositions; the eight groups of Chinese roses have the same growth period and are in the southern plum rain season, 100 Chinese roses are adopted in each group of test, the composition is sprayed once every seven days, and the compositions are continuously applied for three times; observing the change of each group of Chinese roses; and recording the leaf fall amount and bud germination amount of yellow leaves in each group of Chinese roses, and dividing the leaf fall amount of the yellow leaves in each group by the total amount of the Chinese roses to obtain the leaf fall rate of the yellow leaves; dividing the bud germination rate of each group by the total weight of each group of Chinese roses to obtain the bud germination rate; the leaf fall rate and bud germination rate of each group of Chinese rose yellow leaves are shown in table 3:
table 3: change of Chinese rose in plum rain season
Yellow leaf falling rate (%) Bud germination rate (%)
Control group 80 20
Example 1 9.1 85.2
Example 2 7.2 87.7
Example 3 5.5 89.1
Example 4 2.8 90.9
Comparative example 1 15.2 75.9
Comparative example 2 12.3 78.2
Comparative example 3 11.5 79.1
The results in table 3 show that the compositions containing sasanquasaponin as a main ingredient for preventing and treating rosa chinensis diseases prepared in examples 1 to 4 have an obvious effect of inhibiting the phenomenon of yellow leaf defoliation in plum rain season and promoting bud germination; promote the Chinese rose to be luxuriant and leafy.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the technical scope of the present invention.

Claims (10)

1. A composition which is used for preventing and treating diseases of Chinese roses and takes sasanquasaponin as a main component is characterized by comprising the following components: the bacteriostatic agent comprises 5-8 parts by mass of camellia saponin, 1-2.5 parts by mass of orange peel flavone and 1-2.5 parts by mass of anthraquinone bacteriostatic agent; the anthraquinone bacteriostatic agent comprises rhein, aloe-emodin, chrysophanol glucoside, emodin glucoside, physcion glucoside and chrysophanol.
2. The composition taking camellia saponin as a main component for preventing and treating monthly rose diseases according to claim 1, wherein the camellia saponin, the tangerine peel flavone and the anthraquinone bacteriostatic agent are added in a mass part ratio of 8:1: 1; the anthraquinone bacteriostatic agent comprises the following components in percentage by weight: rhein 20-30 wt%, aloe-emodin 10-15 wt%, emodin 15-20 wt%, chrysophanol glucoside 12-18 wt%, emodin glucoside 16-20 wt%, physcion glucoside 5-8 wt% and chrysophanol 13-15 wt%.
3. A method for preparing the composition containing sasanquasaponin as a main component for controlling rose diseases according to any one of claims 1 to 2, characterized in that: the method comprises the following steps:
firstly, preparing sasanquasaponin: crushing raw material camellia oleifera, adding purified water into the crushed raw material camellia oleifera, performing heating reflux extraction for 2.5 to 3.5 hours at the temperature of 95 to 100 ℃, filtering to obtain camellia saponin extraction filtrate, and concentrating the camellia saponin extraction filtrate until the solid content is 10 to 20 percent to obtain camellia saponin concentrated solution;
secondly, preparing orange peel flavone: crushing orange peel, and performing ultrasonic extraction, filtration and reduced pressure concentration on the crushed orange peel powder to obtain an orange peel flavone crude extract; purifying the crude orange peel flavone extract by using a polyamide resin column, eluting by using 40-80% ethanol as an eluent, wherein the volume ratio of orange peel mass to ethanol is 1: 10-1: 60g/mL, so as to obtain an orange peel flavone extract;
thirdly, preparing anthraquinone bacteriostat: pulverizing radix et rhizoma Rhei into coarse powder, extracting with water under reflux, filtering, and mixing filtrates; concentrating the combined filtrate under reduced pressure to obtain water extract concentrated solution, and adding 30% -80% ethanol, heating and reflux extracting to obtain chrysophanol concentrated solution; separating and purifying the chrysophanol concentrated solution by adopting macroporous adsorption resin to obtain anthraquinone bacteriostats of each component;
fourthly, preparation of the composition: dissolving the camellia saponin concentrated solution, the orange peel flavone extract and the anthraquinone bacteriostatic agent in water, stirring and uniformly mixing to obtain a mixed solution, and concentrating the mixed solution under reduced pressure to obtain a composition concentrated solution;
and fifthly, adjusting the pH value of the mixed solution to be 5-6, and then carrying out ultrasonic treatment or stirring to obtain the composition which is used for preventing and treating the diseases of the Chinese roses and takes the sasanquasaponin as a main component.
4. The preparation method of a composition containing camellia saponin as a main component for controlling rose diseases according to claim 3, characterized in that, in the first step, raw camellia oleifera is pulverized to 10-30 mesh, and purified water is added to the pulverized raw camellia oleifera in an amount of 7-9 times the mass of the raw camellia oleifera; the temperature at which the extraction was carried out under heating and refluxing was 98 ℃.
5. The preparation method of the composition containing camellia saponin as a main component for preventing and treating the diseases of roses according to claim 3, wherein the ultrasonic extraction process in the second step is as follows: the ultrasonic power is 500-600W, and the ultrasonic extraction temperature is 60-70 ℃.
6. The method for preparing a composition containing sasanquasaponin as a main component for controlling rose diseases according to claim 3, wherein the conditions of the concentration under reduced pressure in the second step are: under the vacuum of-0.2 MPa, the rotating speed is 110-1150 rpm/min, and the evaporation temperature is 45-48 ℃.
7. The preparation method of a composition containing sasanquasaponin as a main component for controlling rose diseases according to claim 3, wherein the polyamide resin column in the second step is eluted with 65% to 70% ethanol.
8. The method for preparing a composition containing sasanquasaponin as a main component for preventing and treating rose diseases according to claim 3, wherein in the third step, the eluate for separating and purifying the chrysophanol concentrated solution by using macroporous adsorption resin is 30-95% ethanol.
9. The method for preparing a composition containing camellia saponin as a main ingredient for controlling rose diseases according to claim 3, wherein the camellia saponin concentrate, the tangerine peel flavone extract and the anthraquinone bacteriostatic agent are dissolved in water and heated at 70-80 ℃ for 30min to obtain a mixed solution in step four.
10. The preparation method of a composition containing sasanqua saponin as a main ingredient for controlling rose diseases according to claim 3, wherein the pH in the fifth step is adjusted using citric acid-sodium bicarbonate, and the pH is 6.
CN202210627157.1A 2022-06-06 2022-06-06 Composition containing camellia saponin as main component for preventing and treating Chinese rose diseases and preparation method thereof Pending CN114794159A (en)

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