CN113142248A - Pond cleaning agent for aquaculture and preparation method thereof - Google Patents
Pond cleaning agent for aquaculture and preparation method thereof Download PDFInfo
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- CN113142248A CN113142248A CN202110440729.0A CN202110440729A CN113142248A CN 113142248 A CN113142248 A CN 113142248A CN 202110440729 A CN202110440729 A CN 202110440729A CN 113142248 A CN113142248 A CN 113142248A
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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Abstract
The invention provides a pond cleaning agent for aquaculture and a preparation method thereof, and belongs to the technical field of pond cleaning agents. The pond cleaning agent for aquaculture comprises the following components in parts by weight: 56-100 parts of plant extract, wherein the plant extract is a mixture of a fiveleaf gynostemma herb extract, a polygala root extract, a platycodon root extract, a pokeberry root extract and a safflower oxalis extract, and the mass ratio of the fiveleaf gynostemma herb extract, the polygala root extract, the platycodon root extract, the pokeberry root extract and the safflower oxalis extract is (18-34): (12-20): (10-16): (5-11): (11-19); 1-5 parts of tea saponin; 0.014-0.086 part of xanthan gum; 6-43 parts of water. The pond cleaning agent for aquaculture can effectively clean wild trash fishes, snails and other animals in the pond, can inhibit various pathogenic bacteria, has good pond cleaning effect, and can provide a good growth environment for aquaculture animals.
Description
Technical Field
The invention relates to the technical field of pond cleaning agents, in particular to a pond cleaning agent for aquaculture and a preparation method thereof.
Background
The pond is a place where the aquaculture animals inhabit and is also a storage place for various pathogens, the pond is cleaned by adopting a pond cleaning agent before aquaculture, sludge is eliminated, harmful fishes and insects are killed, and the like are one of important links in aquaculture, and the development of pond cleaning work can provide a good living environment for the aquaculture animals and ensure the healthy growth of the aquaculture animals. The drug pond cleaning is an important measure for eliminating wild trash fish and other wild animals, plants and pathogens, and is also the most important pond cleaning method.
The common pond cleaning agents at present comprise chemical pond cleaning agents, pesticide pond cleaning agents and plant pond cleaning agents. The chemical pond cleaning agent mainly comprises lime hydrate, bleaching powder, ammonia water and the like, but the method has the defects of unstable pond cleaning effect, inconvenient storage and use of the pond cleaning agent and high cost. The pesticide pond cleaning agent mainly comprises pesticides (such as pyrethrin pesticides, organophosphorus pesticides and the like) and molluscicides (such as sodium pentachlorophenate, nicotinanilide, niclosamide and the like), and the pond cleaning agent is expensive, easily pollutes the environment and is easily harmful to human bodies and animals. The plant pond cleaning agent is mainly tea meal, and the method is environment-friendly and safe, but fish killing is not thorough and needs to be matched with other medicines for use.
Disclosure of Invention
The invention aims to provide a pond cleaning agent for aquaculture and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a pond cleaning agent for aquaculture, which comprises the following components in parts by weight:
56-100 parts of plant extract, wherein the plant extract is a mixture of a fiveleaf gynostemma herb extract, a polygala root extract, a platycodon root extract, a pokeberry root extract and a safflower oxalis extract, and the mass ratio of the fiveleaf gynostemma herb extract, the polygala root extract, the platycodon root extract, the pokeberry root extract and the safflower oxalis extract is (18-34): (12-20): (10-16): (5-11): (11-19);
1-5 parts of tea saponin;
0.014-0.086 part of xanthan gum;
6-43 parts of water.
Preferably, the plant extracts including the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract and the pokeberry root extract are prepared from corresponding plant raw materials by an independent water extraction and alcohol precipitation method.
Preferably, the water extraction and alcohol precipitation method comprises the following steps:
decocting the plant material powder with water, and performing solid-liquid separation to obtain a first extractive solution;
carrying out first concentration on the first extracting solution to obtain a concentrated solution;
settling the concentrated solution with an ethanol water solution, and performing solid-liquid separation to obtain a second extracting solution;
and carrying out second concentration on the second extracting solution to obtain the extract of the corresponding plant raw material.
Preferably, the particle size of the plant raw material powder is 20-60 meshes; the decocting times are 2-4 times, the mass of water used for each time of decoction is 10-20 times of that of the solid materials, and the time for each time of decoction is 1-1.5 hours;
preferably, the first concentration is carried out under the conditions that the pressure is 0.01-0.05 MPa and the temperature is 50-70 ℃, and the concentration multiple of the first concentration is 18-22 times;
the volume fraction of the ethanol aqueous solution is 80-90%, and the mass ratio of the ethanol aqueous solution to the concentrated solution is (60-90): (8-23); the settling temperature is 20-30 ℃, and the settling time is 2-3 h;
and the second concentration is carried out under the conditions that the pressure is 0.01-0.03 MPa and the temperature is 45-55 ℃, and the second concentration is to concentrate the second extracting solution to be in an extract shape.
Preferably, the safflower oxalis extract in the plant extract is prepared by grinding and extracting safflower oxalis by an ethanol method.
Preferably, the ethanol trituration extraction process comprises the steps of:
grinding the safflower creeping oxalis, and performing solid-liquid separation to obtain a first liquid material;
mixing the first liquid material with an ethanol water solution, extracting, and carrying out solid-liquid separation to obtain a second liquid material;
and concentrating the second liquid material to obtain the safflower oxalis extract.
Preferably, the grinding is to grind the safflower oxalis till the obtained juice completely passes through a 20-60 mesh screen.
Preferably, the volume fraction of the ethanol aqueous solution is 80-90%, and the mass ratio of the ethanol aqueous solution to the first liquid material is (60-95): (8-23); the extraction temperature is 20-30 ℃, and the extraction time is 1-2 h;
the concentration is to concentrate the second liquid material into an extract shape.
The invention provides a preparation method of a pond cleaning agent for aquaculture, which comprises the following steps:
mixing xanthan gum with water to obtain xanthan gum aqueous solution;
and mixing the xanthan gum aqueous solution, the plant extract and the tea saponin to obtain the pond cleaning agent for aquaculture.
The invention provides a pond cleaning agent for aquaculture, which comprises the following components in parts by weight: 56-100 parts of plant extract, wherein the plant extract is a mixture of a fiveleaf gynostemma herb extract, a polygala root extract, a platycodon root extract, a pokeberry root extract and a safflower oxalis extract, and the mass ratio of the fiveleaf gynostemma herb extract, the polygala root extract, the platycodon root extract, the pokeberry root extract and the safflower oxalis extract is (18-34): (12-20): (10-16): (5-11): (11-19); 1-5 parts of tea saponin; 0.014-0.086 part of xanthan gum; 6-43 parts of water. The pond cleaning agent for aquaculture can effectively clean wild trash fishes, snails and other animals in the pond, can inhibit various pathogenic bacteria, has a good pond cleaning effect, and can provide a good growth environment for aquaculture animals. Specifically, the pond cleaning agent for aquaculture provided by the invention takes plant extracts as main components, wherein the gynostemma pentaphyllum extract, the polygala tenuifolia extract and the platycodon grandiflorum extract contain various saponins, so that the pond cleaning agent has a strong hemolytic effect and can effectively remove wild fishes and other animals in a pond; the pokeberry root extract and the safflower oxalis extract also contain saponin, and also contain ferulic acid, rutin, chalcone, dihydrokaempferide, veratrine and other components, and have good effect on removing snails in the pond; the tea saponin contains magnolol and other components, has a certain inhibiting effect on bacillus subtilis and the like, also has the effect of resisting pathogenic microorganisms, and can improve the surface activity of the pool cleaning agent for aquaculture by utilizing the foamability and the dispersibility of the agent, so that the agent can quickly and uniformly diffuse in a pool, the pool cleaning effect can be improved, and the pool cleaning efficiency can be improved; the addition of a small amount of xanthan gum is beneficial to improving the stability of the pond cleaning agent for aquaculture in a liquid phase system during the use process, so that each component can better play a role.
In addition, the components in the pond cleaning agent for aquaculture are cheap and easily available, are all natural and environment-friendly substances, are harmless to human bodies and animals, and have small influence on the environment.
Drawings
FIG. 1 is a graph showing the effect of the pond cleaning agent prepared in example 1;
FIG. 2 is a graph showing the effect of the pond cleaning agent prepared in example 2;
fig. 3 is a diagram showing the pond-cleaning effect of the pond-cleaning agent prepared in example 3.
Detailed Description
The invention provides a pond cleaning agent for aquaculture, which comprises the following components in parts by weight:
56-100 parts of plant extract, wherein the plant extract is a mixture of a fiveleaf gynostemma herb extract, a polygala root extract, a platycodon root extract, a pokeberry root extract and a safflower oxalis extract, and the mass ratio of the fiveleaf gynostemma herb extract, the polygala root extract, the platycodon root extract, the pokeberry root extract and the safflower oxalis extract is (18-34): (12-20): (10-16): (5-11): (11-19);
1-5 parts of tea saponin;
0.014-0.086 part of xanthan gum;
6-43 parts of water.
The pond cleaning agent for aquaculture comprises, by mass, 56-100 parts of plant extracts, preferably 70-80 parts; the plant extract is a mixture of a fiveleaf gynostemma herb extract, a polygala root extract, a platycodon root extract, a poke root extract and a safflower oxalis extract, and the mass ratio of the fiveleaf gynostemma herb extract, the polygala root extract, the platycodon root extract, the pokeberry root extract and the safflower oxalis extract is (18-34): (12-20): (10-16): (5-11): (11-19), preferably (20-30): (15-18): (12-14): (7-9): (13-17). The pond cleaning agent for aquaculture provided by the invention takes plant extracts as main components, wherein the gynostemma pentaphylla extract, the polygala tenuifolia extract and the platycodon grandiflorum extract contain various saponins, so that the pond cleaning agent has a very strong hemolytic effect and can effectively remove animals such as wild fishes and the like in a pond; the pokeberry root extract and the safflower oxalis extract also contain saponin, and also contain ferulic acid, rutin, chalcone, dihydrokaempferide, veratrine and other components, and have good effect on removing snails in the pond. The present invention will be described in detail with respect to the preparation of each extract.
Based on the mass parts of the plant extracts, the pond cleaning agent for aquaculture comprises 1-5 parts of tea saponin. The tea saponin powder is preferably adopted, and the purity of the tea saponin powder is preferably more than or equal to 99 wt%. In the invention, the tea saponin powder contains magnolol and other components, has a certain inhibition effect on bacillus subtilis and the like, and also has an anti-pathogenic microorganism effect. Meanwhile, when the pond cleaning agent for aquaculture is used, the concentration of tea saponin in a water body is preferably 0.001-2.0 mg/L and is far less than the effective fish killing concentration of the tea saponin of 6.74mg/L on the basis of a pond with the depth of 0.5 m/mu, so that the small amount of tea saponin added into the pond cleaning agent for aquaculture does not have fish killing activity; the invention can improve the surface activity of the pool cleaning agent for aquaculture by utilizing the foamability and the dispersibility of the bacillus subtilis on the basis of ensuring the bacillus subtilis inhibiting effect and the pathogenic microorganism resisting effect, so that the bacillus subtilis can quickly and uniformly diffuse in a pond, the pool cleaning effect can be improved, and the pool cleaning efficiency can be improved.
Based on the mass parts of the plant extracts, the pond cleaning agent for aquaculture comprises 0.014-0.086 parts of xanthan gum, and preferably 0.02-0.04 parts of xanthan gum. The invention adopts a small amount of xanthan gum, which is beneficial to improving the stability of the pond cleaning agent for aquaculture in a liquid phase system during the use process, so that each component can better play a role.
Based on the mass parts of the plant extracts, the pond cleaning agent for aquaculture comprises 6-43 parts of water, and preferably 10-20 parts of water.
The method for preparing the plant extract of the present invention will be described in detail below.
In the present invention, the plant extracts, including the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract and the pokeberry root extract, are preferably prepared from the corresponding plant raw materials by an independent water extraction and alcohol precipitation method.
In the present invention, the water extraction and alcohol precipitation method preferably comprises the following steps:
decocting the plant material powder with water, and performing solid-liquid separation to obtain a first extractive solution;
carrying out first concentration on the first extracting solution to obtain a concentrated solution;
settling the concentrated solution with an ethanol water solution, and performing solid-liquid separation to obtain a second extracting solution;
and carrying out second concentration on the second extracting solution to obtain the extract of the corresponding plant raw material.
The invention is characterized in that plant raw material powder is decocted by water, and a first extracting solution is obtained by solid-liquid separation. In the invention, the granularity of the plant raw material powder is preferably 20-60 meshes; preferably, the plant raw materials are dried in a ventilated place and are crushed to 20-60 meshes by a crusher to obtain raw material powder. In the invention, the number of times of decoction is preferably 2-4 times, and more preferably 3 times; the mass of water used for each decoction is preferably 10-20 times of the mass of solid materials (specifically plant raw material powder or solid materials obtained after last decoction), and specifically may be 10 times, 15 times or 20 times; the time for each decoction is preferably 1-1.5 h, and specifically can be 1h, 1.25h or 1.5 h. In the invention, the plant raw material powder is mixed with water, heated to boiling and decocted; then carrying out solid-liquid separation on the obtained system to obtain a liquid material and a solid material, and carrying out next decoction on the solid material by using water according to the method; the time of each decoction is counted as the boiling of the system; and finally, mixing liquid materials obtained by solid-liquid separation after each decoction to obtain a first extracting solution. The solid-liquid separation method is not particularly limited, and a solid-liquid separation method known to those skilled in the art, such as filtration, may be used.
After the first extracting solution is obtained, the first extracting solution is subjected to first concentration to obtain a concentrated solution. In the invention, the first concentration is preferably carried out under the conditions of pressure of 0.01-0.05 MPa and temperature of 50-70 ℃, the pressure can be 0.01MPa, 0.03MPa or 0.05MPa, and the temperature can be 50 ℃, 60 ℃ or 70 ℃; the concentration multiple of the first concentration is preferably 18-22 times, more preferably 20 times, namely the volume of the concentrated solution is preferably 1/18-1/22 times of the volume of the first extracting solution, more preferably 1/20.
After the concentrated solution is obtained, the concentrated solution is settled by using an ethanol water solution, and a second extracting solution is obtained through solid-liquid separation. In the invention, the volume fraction of the ethanol aqueous solution is preferably 80-90%, and more preferably 85%; the mass ratio of the ethanol water solution to the concentrated solution is preferably (60-90): (8-23), more preferably (60-90): (15-18), more preferably (70-75): (16-17); the temperature of the sedimentation is preferably 20-30 ℃, the sedimentation can be carried out at room temperature, and in the embodiment of the invention, the room temperature is 25 ℃; the settling time is preferably 2-3 h, and specifically can be 2h, 2.5h or 3 h. The solid-liquid separation method is not particularly limited, and a solid-liquid separation method known to those skilled in the art, such as filtration, may be used.
After the second extracting solution is obtained, the second extracting solution is subjected to second concentration to obtain the extract of the corresponding plant raw material. In the invention, the second concentration is preferably carried out under the conditions of pressure of 0.01-0.03 MPa and temperature of 45-55 ℃, the pressure can be 0.01MPa, 0.02MPa or 0.03MPa, and the temperature can be 45 ℃, 50 ℃ or 55 ℃; the second concentration is preferably to concentrate the second extract to an extract state. In the present invention, the ethanol volatilized in the second concentration process may be recovered and reused.
In the invention, the safflower oxalis extract in the plant extract is preferably prepared by ethanol grinding extraction method of safflower oxalis. In the present invention, the ethanol milling extraction method preferably comprises the steps of:
grinding the safflower creeping oxalis, and performing solid-liquid separation to obtain a first liquid material;
mixing the first liquid material with an ethanol water solution, extracting, and carrying out solid-liquid separation to obtain a second liquid material;
and concentrating the second liquid material to obtain the safflower oxalis extract.
The invention grinds safflower creeping oxalis and obtains a first liquid material through solid-liquid separation. In the invention, the grinding is preferably carried out until the obtained juice completely passes through a 20-60-mesh screen. The method preferably cleans fresh safflower creeping oxalis, dries in air, and grinds in a mortar until the juice can pass through a 20-60 mesh screen. The solid-liquid separation method is not particularly limited, and a solid-liquid separation method known to those skilled in the art, such as filtration, may be used.
After the first liquid material is obtained, the first liquid material is mixed with ethanol water solution for extraction, and the second liquid material is obtained through solid-liquid separation. In the invention, the volume fraction of the ethanol aqueous solution is preferably 80-90%, and more preferably 85%; the mass ratio of the ethanol water solution to the first liquid material is preferably (60-95): (8-23), more preferably (60-95): (15-18), more preferably (75-80): (16-17); the extraction temperature is preferably 20-30 ℃, and the extraction can be carried out at room temperature; the extraction time is preferably 1-2 h, and specifically can be 1h, 1.5h or 2 h. In the invention, in the extraction process, the stirring is preferably performed once every 10-15 min, and the duration of each stirring is preferably 20-40 min. In the invention, the solid-liquid separation preferably comprises centrifugation and filtration which are sequentially carried out, specifically, a system obtained after extraction is centrifuged, the rotation speed of the centrifugation is preferably 3500-4500 r/min, and the time is preferably 15-25 min; the supernatant from the centrifugation is then filtered to obtain a second liquid material.
After the second liquid material is obtained, the invention concentrates the second liquid material to obtain the safflower oxalis extract. In the present invention, the concentration is preferably performed by concentrating the second liquid material to form an extract. In the present invention, the concentration is preferably performed in a rotary evaporator, and ethanol volatilized during the concentration may be recovered and reused.
The invention provides a preparation method of a pond cleaning agent for aquaculture, which comprises the following steps:
mixing xanthan gum with water to obtain xanthan gum aqueous solution;
and mixing the xanthan gum aqueous solution, the plant extract and the tea saponin to obtain the pond cleaning agent for aquaculture.
The invention mixes xanthan gum and water to obtain xanthan gum aqueous solution. The method for mixing the xanthan gum and the water is not particularly limited, and the xanthan gum and the water can be uniformly mixed, and can be mixed under the stirring condition.
After the xanthan gum aqueous solution is obtained, the xanthan gum aqueous solution, the plant extract and the tea saponin are mixed to obtain the pond cleaning agent for aquaculture. The method preferably mixes the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract, the pokeberry root extract, the safflower oxalis extract and the tea saponin, and then mixes the obtained mixture with a xanthan gum aqueous solution to obtain the pond cleaning agent for aquaculture.
The method for using the pond cleaning agent for aquaculture is not particularly limited, and can be realized by adopting a using method known by the technical personnel in the field, and specifically, the pond cleaning agent for aquaculture is diluted by water and then is uniformly sprayed in a pond. In the invention, the dosage of the pond cleaning agent for aquaculture is determined according to the variety of the trash fish in the pond, wherein the concentration of the tea saponin in the water body is ensured to be not higher than 6.74 mg/L.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
Example 1
According to the mass parts, the pond cleaning agent for aquaculture provided by the embodiment comprises: 26 parts of gynostemma pentaphyllum extract, 16 parts of polygala tenuifolia extract, 13 parts of platycodon grandiflorum extract, 8 parts of pokeberry root extract, 15 parts of safflower creeping oxalis extract, 2 parts of tea saponin (the purity of the tea saponin is 99 wt%) and 20 parts of xanthan gum aqueous solution with the concentration of 0.2 wt%.
The methods of the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract, the pokeberry root extract and the safflower oxalis extract will be described below.
The preparation method of the gynostemma pentaphylla extract comprises the following steps:
(1) airing the gynostemma pentaphylla in a ventilated place, and crushing the gynostemma pentaphylla into 40 meshes by using a crusher to obtain gynostemma pentaphylla powder;
(2) putting the gynostemma pentaphylla powder obtained in the step (1) into a boiling pot, adding water, heating until the water is boiled, then decocting for 1.25h, filtering to obtain filtrate and filter residue, repeating the above decocting steps on the filter residue, wherein the water used for each decocting is 15 times of the weight of the filter residue, decocting for 3 times in total, and mixing the filtrates obtained by 3 times of decocting to obtain a first extracting solution;
(3) performing first concentration on the first extracting solution in the step (2) under the conditions of pressure of 0.03MPa and temperature of 60 ℃ to obtain a concentrated solution; wherein the concentration multiple is 20 times, that is, the volume of the concentrated solution is 1/20 times of the volume of the first extractive solution;
(4) mixing the concentrated solution obtained in the step (3) with an ethanol water solution with the volume fraction of 85%, wherein the mass ratio of the ethanol water solution to the concentrated solution is 75: 16, standing for 2.5 hours at room temperature (25 ℃) after uniformly stirring, and filtering to obtain filtrate as a second extracting solution;
(5) performing second concentration on the second extracting solution in the step (4) under the conditions that the pressure is 0.02MPa and the temperature is 50 ℃ to remove the solvent in the second extracting solution to obtain a pasty gynostemma pentaphyllum extract; and recovering and recycling the ethanol volatilized in the second concentration process.
Referring to the preparation method of the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract and the pokeberry root extract are respectively prepared, and the difference is only that the polygala tenuifolia extract, the platycodon grandiflorum extract and the pokeberry root extract are respectively used as raw materials.
The preparation method of the safflower creeping oxalis extract comprises the following steps:
(a) cleaning fresh safflower creeping oxalis, drying, grinding in a mortar until the juice can pass through a 60-mesh steel wire screen, stopping grinding, and filtering the obtained juice to obtain a first liquid material;
(b) mixing the first liquid material in the step (a) with an ethanol water solution with the volume fraction of 85%, wherein the mass ratio of the ethanol water solution to the first liquid material is 80: 17, standing at room temperature for 1.5h, and stirring once every 10min in the standing process, wherein the duration of each stirring is 20 min; after the placing step is finished, centrifuging the obtained system for 20min at the rotating speed of 4000r/min, and filtering the supernatant obtained by centrifuging to obtain a second liquid material;
(c) carrying out rotary evaporation on the second liquid material in the step (b) in a rotary evaporator to obtain an extract-shaped safflower oxalis extract; and recovering and recycling the ethanol volatilized in the rotary evaporation process.
After the extracts are prepared according to the method, according to the formula of the pond cleaning agent for aquaculture, the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract, the pokeberry root extract, the safflower oxalis extract, the tea saponin (the purity of the tea saponin is 99 wt%) and a xanthan gum aqueous solution with the concentration of 0.2 wt% are added into a mixing container, and the pond cleaning agent for aquaculture is obtained by stirring and mixing uniformly.
The pond cleaning agent prepared in the embodiment 1 of the invention is used for a culture test, and the method comprises the following specific steps:
the breeding test is provided with 3 test groups and 1 control group, wherein the 3 test groups are respectively a test group A, a test group B and a test group C; preparing 4 containers A, B, C and D, 50L of water being added to each container, container A, B, C and container D corresponding to test group A, test group B, test group C and control group, respectively; 0.1g, 0.2g and 0.4g of the pond cleaning agent prepared in example 1 are respectively added into containers A, B and C to obtain pond cleaning agent aqueous solutions with the concentrations of 2mg/L, 4mg/L and 8mg/L, and the pond cleaning agent is not used in a control group; 100 loach, finless eel, carp, grouper and weever seedlings with the same variety and similar size are prepared, the seedlings are averagely divided into 4 groups, 25 seedlings are put into 4 containers respectively, and the mortality rate of the seedlings is observed after 48 hours.
Fig. 1 is a diagram showing the pond-cleaning effect of the pond-cleaning agent prepared in example 1. As can be seen from figure 1, after the pond cleaning agent prepared in example 1 is used for 48 hours, the death rate of each fry of a test group is far higher than that of a control group, the death rate of each fry of the control group is 0, the death rate of each fry of a test group B (the use concentration is 4mg/L) is higher than that of a test group A (the use concentration is 2mg/L), and the difference between the death rate of each fry of the test group B and that of a test group C (the use concentration is 8mg/L) is not great, so that the pond cleaning agent disclosed by the invention can achieve a good pond cleaning effect on wild trash fish.
Example 2
According to the mass parts, the pond cleaning agent for aquaculture provided by the embodiment comprises: 34 parts of gynostemma pentaphyllum extract, 12 parts of polygala tenuifolia extract, 16 parts of platycodon grandiflorum extract, 5 parts of pokeberry root extract, 11 parts of safflower creeping oxalis extract, 3 parts of tea saponin (the purity of the tea saponin is 99 wt%) and 19 parts of xanthan gum aqueous solution with the concentration of 0.2 wt%.
The methods of the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract, the pokeberry root extract and the safflower oxalis extract will be described below.
The preparation method of the gynostemma pentaphylla extract comprises the following steps:
(1) airing the gynostemma pentaphylla in a ventilated place, and crushing the gynostemma pentaphylla into 20 meshes by using a crusher to obtain gynostemma pentaphylla powder;
(2) putting the gynostemma pentaphylla powder obtained in the step (1) into a boiling pot, adding water, heating until the water is boiled, then decocting for 1h, filtering to obtain filtrate and filter residue, repeating the above decocting steps on the filter residue, wherein the water used in each decocting step is 10 times of the mass of the filter residue, decocting for 3 times in total, and mixing the filtrates obtained in the 3 decocting steps to obtain a first extracting solution;
(3) performing first concentration on the first extracting solution in the step (2) under the conditions of pressure of 0.01MPa and temperature of 50 ℃ to obtain a concentrated solution; wherein the concentration multiple is 20 times, that is, the volume of the concentrated solution is 1/20 times of the volume of the first extractive solution;
(4) mixing the concentrated solution obtained in the step (3) with an ethanol water solution with the volume fraction of 85%, wherein the mass ratio of the ethanol water solution to the concentrated solution is 60: 17, standing for 2 hours at room temperature (25 ℃) after uniformly stirring, and filtering to obtain filtrate as a second extracting solution;
(5) performing second concentration on the second extracting solution in the step (4) under the conditions that the pressure is 0.01MPa and the temperature is 45 ℃ to remove the solvent in the second extracting solution to obtain a pasty gynostemma pentaphyllum extract; and recovering and recycling the ethanol volatilized in the second concentration process.
Referring to the preparation method of the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract and the pokeberry root extract are respectively prepared, and the difference is only that the polygala tenuifolia extract, the platycodon grandiflorum extract and the pokeberry root extract are respectively used as raw materials.
The preparation method of the safflower creeping oxalis extract comprises the following steps:
(a) cleaning fresh safflower creeping oxalis, drying, grinding in a mortar until the juice can pass through a 20-mesh steel wire screen, stopping grinding, and filtering the obtained juice to obtain a first liquid material;
(b) mixing the first liquid material in the step (a) with an ethanol water solution with the volume fraction of 85%, wherein the mass ratio of the ethanol water solution to the first liquid material is 60: 17, standing at room temperature for 1h, and stirring once every 10min in the standing process, wherein the stirring duration time is 30 min; after the placing step is finished, centrifuging the obtained system for 15min at the rotating speed of 3500r/min, and filtering the supernatant obtained by centrifuging to obtain a second liquid material;
(c) carrying out rotary evaporation on the second liquid material in the step (b) in a rotary evaporator to obtain an extract-shaped safflower oxalis extract; and recovering and recycling the ethanol volatilized in the rotary evaporation process.
After the extracts are prepared according to the method, according to the formula of the pond cleaning agent for aquaculture, the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract, the pokeberry root extract, the safflower oxalis extract, the tea saponin (the purity of the tea saponin is 99 wt%) and a xanthan gum aqueous solution with the concentration of 0.2 wt% are added into a mixing container, and the pond cleaning agent for aquaculture is obtained by stirring and mixing uniformly.
The pond cleaning agent prepared in example 2 of the present invention was subjected to a culture test according to the method of example 1, and the results are shown in fig. 2. As can be seen from fig. 2, after the pond cleaning agent prepared in example 2 is used for 48 hours, the death rate of each fry in a test group is far higher than that of a control group, and the death rate of each fry in the control group is 0, so that the pond cleaning agent disclosed by the invention can play a good pond cleaning effect on wild trash fish.
Example 3
According to the mass parts, the pond cleaning agent for aquaculture provided by the embodiment comprises: 18 parts of gynostemma pentaphyllum extract, 20 parts of polygala tenuifolia extract, 10 parts of platycodon grandiflorum extract, 11 parts of pokeberry root extract, 19 parts of safflower creeping oxalis extract, 5 parts of tea saponin (the purity of the tea saponin is 99 wt%) and 17 parts of xanthan gum aqueous solution with the concentration of 0.2 wt%.
The methods of the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract, the pokeberry root extract and the safflower oxalis extract will be described below.
The preparation method of the gynostemma pentaphylla extract comprises the following steps:
(1) airing the gynostemma pentaphylla in a ventilated place, and crushing the gynostemma pentaphylla into 60 meshes by using a crusher to obtain gynostemma pentaphylla powder;
(2) putting the gynostemma pentaphylla powder obtained in the step (1) into a boiling pot, adding water, heating until the water is boiled, then decocting for 1.5h, filtering to obtain filtrate and filter residue, repeating the above decocting steps on the filter residue, wherein the water used for each decocting is 20 times of the weight of the filter residue, decocting for 3 times in total, and mixing the filtrates obtained by 3 times of decocting to obtain a first extracting solution;
(3) performing first concentration on the first extracting solution in the step (2) under the conditions of pressure of 0.05MPa and temperature of 70 ℃ to obtain a concentrated solution; wherein the concentration multiple is 20 times, that is, the volume of the concentrated solution is 1/20 times of the volume of the first extractive solution;
(4) mixing the concentrated solution obtained in the step (3) with an ethanol water solution with the volume fraction of 85%, wherein the mass ratio of the ethanol water solution to the concentrated solution is 90: 17, standing for 3 hours at room temperature (25 ℃) after uniformly stirring, and filtering to obtain filtrate as a second extracting solution;
(5) performing second concentration on the second extracting solution in the step (4) under the conditions that the pressure is 0.03MPa and the temperature is 55 ℃ to remove the solvent in the second extracting solution to obtain a pasty gynostemma pentaphyllum extract; and recovering and recycling the ethanol volatilized in the second concentration process.
Referring to the preparation method of the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract and the pokeberry root extract are respectively prepared, and the difference is only that the polygala tenuifolia extract, the platycodon grandiflorum extract and the pokeberry root extract are respectively used as raw materials.
The preparation method of the safflower creeping oxalis extract comprises the following steps:
(a) cleaning fresh safflower creeping oxalis, drying, grinding in a mortar until the juice can pass through a 40-mesh steel wire screen, stopping grinding, and filtering the obtained juice to obtain a first liquid material;
(b) mixing the first liquid material in the step (a) with an ethanol water solution with the volume fraction of 85%, wherein the mass ratio of the ethanol water solution to the first liquid material is 95: 16, standing at room temperature for 2h, and stirring once every 10min in the standing process, wherein the stirring duration time is 40 min; after the placing step is finished, centrifuging the obtained system for 25min at the rotating speed of 4500r/min, and filtering the supernatant obtained by centrifuging to obtain a second liquid material;
(c) carrying out rotary evaporation on the second liquid material in the step (b) in a rotary evaporator to obtain an extract-shaped safflower oxalis extract; and recovering and recycling the ethanol volatilized in the rotary evaporation process.
After the extracts are prepared according to the method, according to the formula of the pond cleaning agent for aquaculture, the gynostemma pentaphyllum extract, the polygala tenuifolia extract, the platycodon grandiflorum extract, the pokeberry root extract, the safflower oxalis extract, the tea saponin (the purity of the tea saponin is 99 wt%) and a xanthan gum aqueous solution with the concentration of 0.2 wt% are added into a mixing container, and the pond cleaning agent for aquaculture is obtained by stirring and mixing uniformly.
The pond cleaning agent prepared in example 3 of the present invention was subjected to a culture test in accordance with the method of example 1, and the results are shown in FIG. 3. As can be seen from FIG. 3, after the pond cleaning agent prepared in example 3 is used for 48 hours, the death rate of each fry in a test group is far higher than that of a control group, and the death rate of each fry in the control group is 0, which shows that the pond cleaning agent provided by the invention can play a good pond cleaning effect on wild trash fish.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A pond cleaning agent for aquaculture comprises the following components in parts by weight:
56-100 parts of plant extract, wherein the plant extract is a mixture of a fiveleaf gynostemma herb extract, a polygala root extract, a platycodon root extract, a pokeberry root extract and a safflower oxalis extract, and the mass ratio of the fiveleaf gynostemma herb extract, the polygala root extract, the platycodon root extract, the pokeberry root extract and the safflower oxalis extract is (18-34): (12-20): (10-16): (5-11): (11-19);
1-5 parts of tea saponin;
0.014-0.086 part of xanthan gum;
6-43 parts of water.
2. The pond cleaning agent for aquaculture according to claim 1, wherein the plant extracts of gynostemma pentaphyllum, polygala tenuifolia, platycodon grandiflorum and pokeberry root are prepared from corresponding plant raw materials by water extraction and alcohol precipitation independently.
3. The pond cleaning agent for aquaculture according to claim 2, wherein the water extraction and alcohol precipitation method comprises the following steps:
decocting the plant material powder with water, and performing solid-liquid separation to obtain a first extractive solution;
carrying out first concentration on the first extracting solution to obtain a concentrated solution;
settling the concentrated solution with an ethanol water solution, and performing solid-liquid separation to obtain a second extracting solution;
and carrying out second concentration on the second extracting solution to obtain the extract of the corresponding plant raw material.
4. The pond cleaning agent for aquaculture according to claim 3, wherein the particle size of the plant raw material powder is 20-60 meshes; the decocting times are 2-4 times, the mass of water used for each time of decoction is 10-20 times of that of solid materials, and the time for each time of decoction is 1-1.5 hours.
5. The pond cleaning agent for aquaculture according to claim 3 or 4, wherein the first concentration is carried out under the conditions of pressure of 0.01-0.05 MPa and temperature of 50-70 ℃, and the concentration multiple of the first concentration is 18-22 times;
the volume fraction of the ethanol aqueous solution is 80-90%, and the mass ratio of the ethanol aqueous solution to the concentrated solution is (60-90): (8-23); the settling temperature is 20-30 ℃, and the settling time is 2-3 h;
and the second concentration is carried out under the conditions that the pressure is 0.01-0.03 MPa and the temperature is 45-55 ℃, and the second concentration is to concentrate the second extracting solution to be in an extract shape.
6. The pond cleaning agent for aquaculture as claimed in claim 1, wherein the plant extract is prepared from safflower oxalis by ethanol milling extraction method.
7. The pond cleaning agent for aquaculture according to claim 6, wherein the ethanol grinding extraction method comprises the following steps:
grinding the safflower creeping oxalis, and performing solid-liquid separation to obtain a first liquid material;
mixing the first liquid material with an ethanol water solution, extracting, and carrying out solid-liquid separation to obtain a second liquid material;
and concentrating the second liquid material to obtain the safflower oxalis extract.
8. The pond cleaning agent for aquaculture according to claim 7, wherein the grinding is carried out by grinding the safflower oxalis till the obtained juice completely passes through a 20-60 mesh screen.
9. The pond cleaning agent for aquaculture according to claim 7 or 8, wherein the volume fraction of the ethanol aqueous solution is 80-90%, and the mass ratio of the ethanol aqueous solution to the first liquid material is (60-95): (8-23); the extraction temperature is 20-30 ℃, and the extraction time is 1-2 h;
the concentration is to concentrate the second liquid material into an extract shape.
10. A method for preparing a pond cleaning agent for aquaculture according to any one of claims 1 to 9, comprising the following steps:
mixing xanthan gum with water to obtain xanthan gum aqueous solution;
and mixing the xanthan gum aqueous solution, the plant extract and the tea saponin to obtain the pond cleaning agent for aquaculture.
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Cited By (1)
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| CN115568469A (en) * | 2022-10-11 | 2023-01-06 | 湖南省林业科学院 | Compound water zooplankton inhibitor of tea saponin, preparation method and application thereof |
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