CN106083765A - A kind of Environmental Safety abluent with antibacterial functions - Google Patents

A kind of Environmental Safety abluent with antibacterial functions Download PDF

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CN106083765A
CN106083765A CN201610363524.6A CN201610363524A CN106083765A CN 106083765 A CN106083765 A CN 106083765A CN 201610363524 A CN201610363524 A CN 201610363524A CN 106083765 A CN106083765 A CN 106083765A
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seaweed
antibacterial
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surfactant
parts
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CN106083765B (en
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石萍
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
    • C07D303/02—Compounds containing oxirane rings
    • C07D303/12—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms
    • C07D303/32—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms by aldehydo- or ketonic radicals
    • 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
    • A01N31/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
    • A01N31/08—Oxygen or sulfur directly attached to an aromatic ring system
    • A01N31/16—Oxygen or sulfur directly attached to an aromatic ring system with two or more oxygen or sulfur atoms directly attached to the same aromatic ring system
    • 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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02—Biocides, 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
    • A01N43/04—Biocides, 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
    • A01N43/20—Biocides, 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 three- or four-membered rings
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
    • C07C37/82—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by solid-liquid treatment; by chemisorption
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/04—Carboxylic acids or salts thereof
    • C11D1/10—Amino carboxylic acids; Imino carboxylic acids; Fatty acid condensates thereof
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/83—Mixtures of non-ionic with anionic compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/88—Ampholytes; Electroneutral compounds
    • C11D1/94—Mixtures with anionic, cationic or non-ionic compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2096—Heterocyclic compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/48—Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/662—Carbohydrates or derivatives

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Abstract

The present invention relates to a kind of there is the Sargassum extract of antibacterial functions, the antibacterial comprising this Sargassum extract, compositions and preparation method thereof, belong to the technical field of antibacterial abluent.The feature of the present composition is containing Sargassum antibacterial, surfactant, antioxidant, water, and especially Sargassum antibacterial is selected from Sargassum extract anion surfactant compound；And disclose corresponding preparation method and purposes.The present invention has environmentally safe, the environmental protection abluent gentle to people's safety, and this is also beneficial to the safe feature of environment and human lives.

Description

Environment-friendly safe cleaning agent with antibacterial function
Technical Field
The invention relates to the technical field of antibacterial cleaning agents, and particularly relates to a seaweed extract with an antibacterial function, a bactericide containing the seaweed extract, a composition containing the seaweed extract and a preparation method of the composition.
Background
In daily life and work, a large amount of bacteria, viruses and other harmful substances are accumulated on the surfaces of electric appliances, furniture, daily necessities used by people and the skin of the human body, and people should use detergents to clean and eliminate the harmful substances frequently, otherwise, the harmful substances threaten the health of the human body. Therefore, it is common to add antibacterial agents to detergents to inhibit the number of bacteria.
Antibacterial agents (anti-bacterial agents) are substances or products having antibacterial and bactericidal properties. Antibacterial agents are generally classified into inorganic antibacterial agents and organic antibacterial agents. Inorganic antibacterial agents are classified into metallic inorganic antibacterial agents and photocatalytic inorganic antibacterial agents according to an antibacterial mechanism. The reagent has high price, antibacterial effect and no effect on mould. Organic antibacterial agents can be classified into synthetic and natural organic antibacterial agents. The synthetic organic antibacterial agent mainly comprises quaternary ammonium salt, quaternary phosphonium salt, organic metal, halogenated amine, biguanide and the like. The synthetic organic antibacterial agent has the advantages of low price, high sterilization speed and wide application, but has the defects of poor heat resistance, easy precipitation in solvents and added matrixes, toxic decomposition products and the like, and a large amount of use causes the bacteria and fungi to gradually generate drug resistance to the bacteria and fungi to influence the antibacterial effect. The natural organic antibacterial agent is the earliest antibacterial agent for human beings, and is an organic substance with antibacterial activity extracted from some animals and plants, such as chitosan and derivatives thereof extracted from crab and shrimp shells, and extracts of mint, lemon leaves and the like. Compared with inorganic and organic synthetic antibacterial agents, the natural antibacterial agent has high use safety, no toxicity or irritation to human bodies, but the existing natural organic antibacterial agent has poor heat resistance and short duration of drug effect.
At present, the organic synthetic antibacterial agent is widely used in various cleaning agents and has the functions of antisepsis, antibiosis and the like. However, since cleaning agents are closely related to human life, their possible toxic effects of oral or transdermal penetration are at all times a threat to human health. Although the molecular structure of natural antibacterial components can be modified and reformed by chemical synthesis to enhance the antibacterial effect and stability of the natural organic antibacterial agents aiming at the defects of the natural organic antibacterial agents, the complex chemical synthesis process necessarily brings the residual risk of other process compounds. Therefore, the naturally extracted antibacterial agent is more suitable for developing safe and non-toxic daily chemical products aiming at sensitive people.
Many cleaning agents in the market adopt surfactants with poor biodegradability, or surfactants containing phosphate can cause eutrophication of water bodies, can cause pollution to soil and water bodies, and seriously harm the environmental health. Numerous medical studies have demonstrated that the surfactants of the alkylsulfonic acid type, which have been widely used, have a strong degreasing and irritating action on the skin, damaging the hair and skin. Therefore, there is a need to develop a green environmental-friendly cleaning agent which has good biodegradability, no pollution to the environment and is safe and mild to human beings, and is also beneficial to the safety of the environment and human life.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a seaweed extract which contains seaweed polyphenol and fucoxanthin. Wherein, the extraction rate of the seaweed polyphenol can be more than 1 percent, such as 2 to 50 percent, 3 to 40 percent and 4 to 20 percent.
According to the present invention, there is no particular limitation on the method for preparing the algal extract as long as it can achieve the algal polyphenol extraction rate defined in the present invention.
As an example, the seaweed extract may be prepared by the following method: extracting the seaweed with one or more of water and an organic solvent as a solvent under ultrasonic conditions.
According to the invention, the seaweed may be Ascophyllum nodosum (Ascophyllum nodosum), Fucus vesiculosus (Fucusiliculosus L), other seaweed or a mixture of two or more seaweed.
According to the invention, the seaweed is pre-treated before extraction. The pretreatment may include soaking and/or pulverizing. Preferably, when the ascophyllum nodosum is extracted using ultrasound, the ascophyllum nodosum is ascophyllum nodosum powder.
According to the preparation method of the invention, the ultrasonic extraction can be ultrasonic cell pulverization extraction.
Preferably, the ultrasonic extraction is performed simultaneously with stirring, e.g. magnetic stirring. For example, the rotation speed of the stirring is 50rpm or more, for example, 100rpm to 500rpm, 200rpm to 400 rpm.
The temperature of the ultrasonic extraction may be below 60 deg.C, preferably below 50 deg.C, such as below 30 deg.C, such as below 10 deg.C.
The ultrasonic extraction time can be more than 5min, for example 10-150 min, preferably 20-90 min, such as 25-60 min, 30-45 min.
Preferably, the ratio of the seaweed material to the solvent may be 1-50 g/100mL of solvent, such as 3-20 g/100mL of solvent, 6-18 g/100mL of solvent, preferably 9-15 g/100mL of solvent, more preferably 12-14 g/100mL of solvent, such as 12.81g/100mL of solvent.
The solvent may be selected from one or more of water, alcohol solvent, ester solvent, and ketone, preferably one or more of methanol, ethanol, propanol, isopropanol, butanol, isobutanol, ethyl acetate, methyl acetate, ethyl formate, methyl formate, and acetone. When a mixture of two solvents is selected as the solvent, the volume ratio of the two solvents may be 10:1 to 1:10, for example, 9:1 to 2: 1.
The ultrasonic power may be 95-855 w, such as 190-665 w, preferably 260-475 w, for example 400 w.
Preferably, the material obtained is also centrifuged or filtered after extraction. Specific conditions for centrifugation are not particularly limited, for example: the temperature can be below 60 deg.C, preferably below 50 deg.C, such as below 30 deg.C, such as below 10 deg.C, such as below 4 deg.C, the rotation speed can be 12,000rpm, 10,000rpm, 8,000rpm, 5,000rpm, and the centrifugation time can be 15min, 10min, 8min, 3 min.
Preferably, the supernatant or filtrate obtained by centrifugation is distilled under reduced pressure and lyophilized.
The invention also provides a seaweed antibacterial agent which is a compound of the seaweed extract and an anionic surfactant (seaweed extract-anionic surfactant compound). Preferably, the seaweed extract-anionic surfactant complex is a synergistic bactericide with synergistic activity.
The invention also provides a preparation method of the seaweed antibacterial agent, which comprises the step of mixing the seaweed extract with the anionic surfactant to obtain the seaweed extract-anionic surfactant compound.
According to the present invention, the anionic surfactant may be selected from one or more of sodium lauroyl sarcosinate, sodium dodecyl sulfate, etc.
According to the preparation method of the present invention, the anionic surfactant may be in the form of an anionic surfactant powder or in the form of an aqueous solution. The concentration of the aqueous solution of the anionic surfactant is not particularly limited, and may be, for example, 1 to 60 vol%, for example, 2 to 40 vol%, or 5 to 20 vol%.
According to the preparation method of the present invention, the ratio of the anionic surfactant to the seaweed extract may be 1 to 8 vol%, preferably 2 to 5 vol%.
The preparation method further comprises the steps of mixing the seaweed extract with the anionic surfactant, standing overnight, precipitating, and removing supernatant to obtain the seaweed extract-anionic surfactant compound.
The invention also provides an algae antibacterial composition which comprises the algae antibacterial agent.
According to the present invention, preferably, the antibacterial active ingredient in the seaweed antibacterial composition is the seaweed antibacterial agent. In other words, the seaweed antimicrobial composition preferably does not contain other antimicrobial agents.
The seaweed antibacterial composition according to the present invention may further optionally comprise one or more of a surfactant, an antioxidant, and water.
According to the present invention, when one or more of the following components of the seaweed antibacterial composition are present, the ratio may be, for example:
more than 0.1 weight part of seaweed antibacterial agent;
1 to 60 parts by weight of a surfactant;
0.05 to 10 parts by weight of antioxidant;
20 to 100 parts by weight of water.
The seaweed antibacterial composition according to the present invention, wherein the seaweed antibacterial agent is preferably 0.5 to 50 parts by weight, for example 1 to 5 parts by weight;
the surfactant may be 1 to 60 parts by weight, preferably 5 to 50 parts by weight, for example 8 to 25 parts by weight;
the antioxidant may be 0.05 to 10 parts by weight, preferably 0.1 to 5 parts by weight, for example 0.2 to 1 part by weight;
the water may be 20 to 100 parts by weight, preferably 30 to 95 parts by weight, for example 50 to 90 parts by weight.
As an example, the seaweed antibacterial composition includes 1.0 to 5.0 parts by weight of a seaweed antibacterial agent; 4 to 50 parts by weight of a surfactant; 0.2 to 1.0 part by weight of antioxidant; and 54-90 parts by weight of water.
According to the invention, the sum of the weight percentages of the components in the seaweed antibacterial composition is 100%.
The antibacterial marine alga composition according to the present invention may preferably be selected from the following group, independently:
the antioxidant is independently selected from ascorbic acid and its sodium salt, erythorbic acid and its sodium salt, natural phytic acid (i.e., phytic acid), Butyl Hydroxy Anisole (BHA), dibutyl hydroxy toluene (BHT) and Propyl Gallate (PG), ethoxyquin, mixed tocopherol concentrate and guaiac resin, lipoic acid, 2, 6-di-tert-butylcresol, ascorbyl palmitate, lauryl thiodipropionate, lecithin, metabisulfite, ascorbyl stearate, amyl gallate, vanillylamide, carnosol, rosmanol, epigallocatechin gallate, epicatechin gallate, catechin, astaxanthin, vitamins, citric acid, carotene, carotenoid, or a combination of two or more thereof;
the surfactant may be a nonionic surfactant and/or an amphoteric surfactant.
When a mixture of nonionic and amphoteric surfactants is used, the weight ratio of the nonionic to amphoteric surfactants can be 10:1 to 1:10, such as 10:1 to 1.5:1, e.g., 5:2, 4:3, 2: 1.
The nonionic surfactant and the amphoteric surfactant are not particularly limited. Wherein,
the nonionic surfactant is independently selected from sorbitan ester, sucrose ester, alkyl glycoside or combination of two or more thereof;
the amphoteric surfactant is independently selected from amino acid surfactant, betaine type amphoteric surfactant, or a combination of two or more thereof.
Preferably, the amino acid surfactant is an alkyl aminopropionate, a hydrochloride salt of an alkyl aminopropionic acid, more preferably a dodecyl aminopropionate, a hydrochloride salt of a dodecyl aminopropionic acid.
The water may be purified water.
According to an embodiment of the present invention, the seaweed antimicrobial composition may be a cleaning agent, for example, may be a dish detergent, a skin detergent, a fruit and vegetable detergent, a laundry detergent.
According to an embodiment of the present invention, the pH of the algal antibacterial composition may be 4.5 to 6.5, preferably 5.0 to 5.9.
According to the present invention, the pH value of the seaweed antibacterial composition can be adjusted by an antioxidant, and can also be adjusted by adding an additional pH adjusting agent. The additional pH adjuster is not particularly limited, and may be, for example, a pH adjuster commonly used in foods or daily chemical products. As an example, the additional pH adjusting agent may be selected from one or more of citric acid, malic acid, tartaric acid, lactic acid, acetic acid, phosphoric acid.
The invention also provides a preparation method of the seaweed antibacterial composition, which comprises the step of mixing the required components of the seaweed antibacterial composition.
According to an embodiment of the method for preparing the antibacterial marine algae composition of the present invention, the method comprises the steps of:
1) mixing the seaweed antibacterial agent with water;
2) mixing a nonionic surfactant with the mixture obtained in step 1);
3) adding an amphoteric surfactant into the mixture obtained in the step 2) and mixing;
4) mixing an antioxidant with the mixture obtained in the step 3) to obtain the seaweed antibacterial composition.
The preparation method according to the present invention may further comprise stirring the mixture in one or more steps above. The stirring time is not particularly limited as long as the mixture can be substantially homogeneous or substantially dissolved, and is preferably homogeneous or sufficiently dissolved. As an example, the stirring time of each step may independently be 5 to 60min, such as 15 to 45min, preferably 30 min.
According to the preparation method of the present invention, the temperature of one or more steps described above may be 50 ℃ or less, for example, 40 ℃ or less. Preferably, the preparation method further comprises controlling the temperature of one or more steps.
According to the preparation method of the present invention, preferably, after the required components of the seaweed antibacterial composition are mixed, the seaweed antibacterial composition is obtained by cooling and defoaming.
The invention also provides a kit comprising the seaweed antibacterial composition of the invention, wherein the seaweed antibacterial composition in the kit is contacted with an inert atmosphere.
According to an embodiment of the present invention, the housing of the kit may be made of metal or engineering plastic. The metal may be aluminum, steel, or an alloy, etc. Preferably, the seaweed antibacterial composition in the kit is in an inert atmosphere.
The invention also provides a cleaning agent containing the seaweed antibacterial composition.
The invention also provides application of the seaweed antibacterial composition in preparing a cleaning agent.
According to the invention, the cleaning agent may be selected from the group consisting of dishwashing, dermatological, fruit and vegetable, laundry detergents. Preferably baby or child bottle or bottle detergents; skin detergent for infant or children such as hand cleanser and face cleanser.
The invention also provides the seaweed antibacterial composition, a seaweed antibacterial agent and an application of the cleaning agent in antibiosis or bacteriostasis.
Term interpretation and description
The features mentioned in the description and the claims of the present invention, including the features exemplified, the exemplary features, the preferred features, the specific features in the embodiments, etc., can be combined and coupled with each other arbitrarily, unless otherwise stated. Such combinations and combinations are within the scope of the present invention.
As will be understood by those skilled in the art, the numerical ranges used herein represent at least the number of significant 1 and significant 2 digits remaining after the recitation of the number of individual integer values and decimal points within the range. For example, a numerical range of 1 to 10 should be understood to describe not only integers wherein 1, 2, 3, 4, 5, 6, 7, 8, 9, 10 are recited, but also all numbers having a numerical size between any two integers and a numerical significance of 1 and 2 remaining after the decimal point.
The term "optionally comprising" as used herein means containing or not containing the recited components.
Advantageous effects
The seaweed antibacterial composition contains the seaweed antibacterial agent, has high-efficiency antibacterial capacity and decontamination capacity, is safe and mild, and is suitable for sensitive people. The antibacterial agent used in the invention is an extract from seaweed, and the extract contains seaweed polyphenol and fucoxanthin, so that the antibacterial agent not only can kill pathogenic bacteria, but also can inhibit the growth of bacteria for a long time. The seaweed extraction process does not need chemical synthesis, and has no risk of other compound residues. The formula uses the non-ionic or amphoteric surfactant with good biodegradability, safety and mildness, and is more suitable for developing safe and non-toxic side effect cleaning agent products aiming at sensitive people.
The seaweed antibacterial agent has excellent sterilization and bacteriostasis functions, is safe and nontoxic, and has no compound residue risk. The amphoteric surfactant and the nonionic surfactant are novel high-quality surfactants, are non-toxic, safe, mild, non-irritant and have good biodegradability. Ascorbic acid is an antioxidant, and in the formula, the pH value of the system can be adjusted, and the seaweed antibacterial component is prevented from losing effectiveness due to oxidation.
The invention utilizes the interaction of sodium lauroyl sarcosine on antibacterial components in seaweed to primarily purify the crude seaweed extract, removes a large amount of water and other seaweed polysaccharides possibly dissolved in water, and forms a precipitate compound, namely the seaweed antibacterial agent. The seaweed antibacterial agent is rich in seaweed antibacterial components, greatly improves the solubility of the seaweed antibacterial components in water, removes other seaweed components which may influence the antibacterial effect, enhances the antibacterial performance and improves the service performance. The microbial sterilization and bacteriostasis effect detection shows that the average sterilization rate of the seaweed antibacterial agent to escherichia coli, candida albicans and staphylococcus aureus is greater than 95%, the average bacteriostasis rate is greater than 95%, and the bacteriostasis time is more than 8 hours. Meanwhile, the safety is higher, and the antibacterial property is better.
Moreover, those skilled in the art will understand that the method of the present invention is not only applicable to the extract obtained by solvent extraction as listed in the examples, but also applicable to the extract obtained by other conventional solvent extraction, as long as the extraction rate of the algal polyphenols meets the definition of the present invention, so that the compound can be formed and good bactericidal and bacteriostatic effects can be obtained.
The advantages of the invention mainly include: 1) the natural antibacterial agent extracted from the seaweed has strong killing and long-acting inhibiting effects on common harmful microorganisms, particularly pathogenic bacteria, and no preservative is required to be added; 2) compared with other natural antibacterial agents added with the molecular structure modification synergy, the method avoids the residual risk of harmful compounds in the chemical synthesis process; 3) the surfactant which is non-toxic, safe, non-irritant, excellent in cleaning performance and harmless to the environment is selected; 4) a low-foam and weakly acidic formula is adopted, so that the washing is convenient; 5) the process flow is simple and convenient; is suitable for sensitive people.
Detailed Description
The following provides a detailed description of the present invention with reference to the corresponding examples. However, it is understood by those skilled in the art that the following examples are not intended to limit the scope of the present invention, and any modifications and variations based on the present invention are within the scope of the present invention.
The experimental procedures described in the following examples are conventional, unless otherwise specified; the materials and reagents are commercially available, unless otherwise specified.
EXAMPLE 1 preparation of seaweed antibacterial agent
1) Preparation method of Sargassum extract
Ascophyllum nodosum (Ascophyllum nodosum) dry powder (100 mesh) was purchased from Stawest Botanicals, Canada.
The 9kg of Ascophyllum nodosum powder is subjected to ultrasonic extraction with 300L of 80% methanol aqueous solution, and ultrasonic cell pulverizer (Ningbo Xinzhi) is adopted, wherein the power of ultrasonic process is 400w, and simultaneously the auxiliary stirring is carried out, the rotating speed is 200rpm, the temperature is controlled below 30 ℃, and the time is 30 min. Centrifuging at 10,000rpm and 4 deg.C for 10min, collecting supernatant, and distilling under reduced pressure to remove solvent to obtain Sargassum extract for use. The seaweed extract contains seaweed polyphenol and fucoxanthin, and the extraction rate of the polyphenol in the seaweed extract is 4% relative to the extraction rate of the seaweed powder.
2) Preparation of seaweed antibacterial agent
Mixing 2kg of seaweed extract with 100L of 5 vol% sodium lauroyl sarcosinate aqueous solution, standing overnight, precipitating, and removing supernatant to obtain seaweed extract-sodium lauroyl sarcosinate compound, i.e. seaweed antibacterial agent.
EXAMPLE 2 preparation of detergent containing seaweed antibacterial agent
1. Adding purified water with the mass 10 times that of the seaweed antibacterial agent prepared in the example 1 into a reaction kettle, adding the seaweed antibacterial agent in the formula proportion, and fully and uniformly stirring, wherein the temperature is controlled below 40 ℃.
2. Adding the nonionic surfactant according to the formula proportion, stirring for 30min, and controlling the temperature below 40 ℃;
3. adding the amphoteric surfactant according to the formula ratio, stirring for 30min, and controlling the temperature below 40 ℃.
4. Dissolving ascorbic acid in the rest purified water, adding, stirring for 30min, and controlling temperature below 40 deg.C.
5. Cooling and defoaming in a storage tank.
6. The obtained product is clear, has no precipitate, has sterilization and bacteriostasis rates of over 90 percent, and is subpackaged.
Example 3 cleaning agent containing seaweed antibacterial agent
2.5g of seaweed antibacterial agent; alkyl glycoside APG 15.0 g; 6.0g of amino acid surfactant; 0.8g of ascorbic acid; purified water 75.7 g.
Example 4 antibacterial, environment-friendly and safe infant hand sanitizer
The basic formula of the cleaning agent is as follows: 3.0g of seaweed antibacterial agent; alkyl glycoside APG 8.0 g; 6.0g of amino acid surfactant; 0.6g of ascorbic acid; purified water 82.4 g.
After the basic formulation of the cleaning agent was completed, 1.0g of a skin moisturizer was added.
Example 5 antibacterial, environmentally friendly and safe fruit and vegetable cleaning agent
The basic formula of the cleaning agent is as follows: 2.0g of seaweed antibacterial agent; alkyl glycoside APG 8.0 g; 4.0g of amino acid surfactant; 0.5g of ascorbic acid; purified water 85.5 g.
Example 6 Activity test
A. Test method
According to the evaluation method of the antibacterial and bacteriostatic effects of QBT 2850-:
1. reagent preparation
1.1 nutrient agar solid Medium
Weighing 10.0g of peptone, 5.0g of beef extract and 5.0g of sodium chloride, adding 1000mL of distilled water for dissolving, adjusting the pH value to 7.2-7.4, adding 15.0g of agar, heating for dissolving, subpackaging, and sterilizing for 20min at 121 ℃ by steam for later use.
1.2 nutrient agar liquid Medium
Weighing 10.0g of peptone, 5.0g of beef extract and 5.0g of sodium chloride, adding 1000mL of distilled water for dissolving, adjusting the pH value to 7.2-7.4, subpackaging, and sterilizing for 20min at 121 ℃ by pressure steam for later use.
1.3 Standard hard Water (hardness 342mg/L)
Weighing calcium chloride (CaCl)2)0.034g, magnesium chloride (MgCl)2.6H2O)0.139g, adding 1000mL of distilled water, sterilizing for 20min at 121 ℃ under steam pressure for later use.
1.4 Phosphate Buffer (PBS) (0.03mol/L)
Weighing 2.83g of anhydrous disodium hydrogen phosphate and 1.36g of monopotassium phosphate, adding 1000mL of distilled water, adjusting the pH value to 7.2-7.4 after complete dissolution, and sterilizing for 20min by using pressure steam at 121 ℃ for later use.
1.5 neutralizing agent
1.36g of monopotassium phosphate, 2.83g of disodium hydrogen phosphate, 3.0g of lecithin, 8020.0 g of tween and 1000mL of distilled water;
1.6 preparation of bacterial liquid
Taking original bacteria liquid of escherichia coli, coating the original bacteria liquid on a solid culture medium, selecting single colony in a region after 24 hours, inoculating the single colony in a liquid culture medium, culturing at 30 ℃ for 18-24 hours to prepare mother liquor, roughly measuring the bacteria content by using a bacteria concentration turbidimetry method, and proposing to use a spectrophotometer with the wavelength of 600nmWavelength, to establish the concentration of bacteria (e.g. 1 × 10)4/1×105/1×106/1×107) The concentration of bacteria can be roughly determined from the curve of absorbance (the concentration of bacteria can be verified by dilution plating), and the concentration of bacteria is preferably 1 × 106～1×107Then diluted by one time, the bacterial concentration is about 5 × 105～5×106. Placing in a refrigerator at 4 ℃ for later use. Should be used on the day, should not be used overnight.
3. The operation steps of the sterilization experiment are as follows:
a) diluting the test bacterial suspension with PBS to a desired concentration, dripping 0.1mL of the test bacterial suspension into 5mL of a control sample solution (PBS), and recovering bacteria with a count of 1 × 104～9×104CFU/mL；
b) Diluting a test sample to a specified concentration of 1:5 by using sterile standard hard water;
c) sucking 5.0mL of test sample diluent, placing the test sample diluent into a sterilization test tube, and keeping the temperature at 20 ℃ for 5 min;
d) sucking 0.1mL of test bacterium liquid, adding the test bacterium liquid into a test tube containing 5.0mL of sample, quickly and uniformly mixing, and immediately timing for 5 min;
e) after the test bacteria and the sample act for a set time, 0.1mL of mixed solution of the test bacteria and the sample is added into a test tube containing 5.0mL of sterilized neutralizer and mixed evenly;
f) after neutralization for 10min, 1mL of the sample solution (or 2-3 dilutions of the sample solution after appropriate dilution) was aspirated and placed in sterile plates, and two sterile plates were inoculated with each sample solution or dilution. Pouring 15mL of nutrient agar solid culture medium (bacteria) cooled to 40-45 ℃, rotating the plate to fully and uniformly, turning the plate after agar is solidified, and counting viable bacterial colonies after culturing for 48 hours (bacteria) at 35 +/-2) DEG C;
g) replacing a test sample with PBS, and simultaneously operating according to the steps to serve as a control sample;
h) the experiment was repeated three times and averaged.
4. Operation procedure of bacteriostatic experiment 1
a) Diluting the test bacterial suspension with PBS to a desired concentration, dripping 0.1mL of the test bacterial suspension into 5mL of a control sample solution (PBS), and recovering bacteria with a count of 1 × 104～9×104CFU/mL；
b) Diluting a test sample to a specified concentration of 1:5 by using sterile standard hard water;
C) sucking 5.0mL of test sample diluent, placing the test sample diluent into a sterilization test tube, and keeping the temperature at 20 ℃ for 5 min;
d) sucking 0.1mL of test bacterium liquid, adding the test bacterium liquid into a test tube containing 5.0mL of a sample, quickly and uniformly mixing, and immediately timing for 5 min;
e) after the test bacteria and the sample are acted for a set time, 0.1mL of mixed solution of the test bacteria and the sample is added into a test tube containing 5.0mL of sterilized PBS and fully and uniformly mixed;
f) after standing for 10min, 1mL of the sample solution (or diluted appropriately, 2-3 dilutions of the sample solution) was aspirated and placed in sterile plates, and two sterile plates were inoculated with each sample solution or dilution. Pouring 15mL of nutrient agar solid culture medium (bacteria) cooled to 40-45 ℃, rotating the plate to fully and uniformly, turning the plate after agar is solidified, culturing for 48 hours (bacteria) at 35 +/-2) ℃, and counting viable bacteria colonies;
g) PBS is used for replacing a test sample, and the following steps are carried out at the same time to be used as a control sample;
h) the experiment was repeated three times and averaged.
5. Bacteriostatic experiment 2 operation steps:
a) diluting the test bacterial suspension with PBS to a desired concentration, dripping 0.1mL of the test bacterial suspension into 5mL of a control sample solution (PBS), and recovering bacteria with a count of 1 × 104～9×104CFU/mL；
b) Sucking 20% or 1% of test sample, placing into a sterilized test tube, adding 50% of nutrient agar liquid culture medium and 30% or 49% of PBS solution, respectively, the total volume is 5mL, mixing, and keeping the temperature at 20 deg.C for 5 min;
c) sucking 0.1mL of test bacterial liquid, adding the test bacterial liquid into the test tube containing 5.0mL of the mixed liquid in the step b, quickly and uniformly mixing, (35 +/-2) DEG C culturing, and immediately timing;
d) after culturing for 5min, 1h, 3h, 5h and 7h respectively, 1mL of sample solution (or diluted appropriately, 2-3 dilutions of the sample solution) is sucked and placed in a sterilized plate, and two sterilized plates are inoculated with each sample solution or dilution. Pouring 15mL of nutrient agar solid culture medium (bacteria) cooled to 40-45 ℃, rotating the plate to fully and uniformly, turning the plate after agar is solidified, culturing for 48 hours (bacteria) at 35 +/-2) ℃, and counting viable bacteria colonies;
e) PBS is used for replacing a test sample, and the following steps are carried out at the same time to be used as a control sample;
f) the experiment was repeated three times and averaged. (ii) a
B test results
Testing bacteria: escherichia coli
Concentration of bacterial liquid 2 × 109CFU/mL
Table 1: bacteriostatic data
Numbering Cleaning agent of example 3 PBS (control)
Number of remaining bacteria 35 1100
Rate of inhibition of bacteria 96.8％ -
Table 2: sterilization data
Numbering Cleaning agent of example 3 PBS (control)
Number of remaining bacteria 15 1075
Rate of sterilization 98.6％ -
Table 3: cleaning agent dilution 1 of example 3: 5 Long-acting bacteriostatic data
Time of action 5min 1h 3h 5h 7h
Number of remaining bacteria 5 3 3 4 5
PBS (control) 116 167 1500 Can not count Can not count
Rate of inhibition of bacteria 95.7％ 98.2％ 99.8％
Table 4: cleaning agent dilution 1 of example 3: 100 long-acting bacteriostatic data
Time of action 5min 1h 3h 5h 7h
Number of remaining bacteria 7 5 5 16 200
PBS (control) 116 167 1500 Can not count Can not count
Rate of inhibition of bacteria 94.0％ 97.0％ 99.7％
In addition, tests show that the sterilization rate and the bacteriostasis rate of the detergents in the examples 4 and 5 are both more than or equal to 90 percent.
Example 7 Activity assays with other seaweed extracts
The inventors also extracted ascophyllum nodosum using an ultrasonic method using other solvents (absolute methanol, absolute ethanol or absolute acetone) and post-treated the extract using a procedure similar to step 1) of example 1, and the extraction rates of algal polyphenols in the obtained extract were about 2%, 1% and 1.5%, respectively. Then, the cleaning agent is prepared by using the method of the step 2) of the embodiment 1 and the methods of the embodiments 2 and 3, and the obtained product is tested for sterilization and bacteriostatic activity, so that the sterilization rate and the bacteriostatic rate are both more than 90%.
Example 8 comparative example of Activity test
Referring to the test method of example 6, replacing the seaweed antibacterial agent in the detergents of examples 3, 4 and 5 with the seaweed extract in step 1) of example 1, the bactericidal and bacteriostatic rates were only in the range of 10-30%, which was much lower than those of the detergents of examples 3, 4 and 5 described in example 6.

Claims (10)

1. A seaweed extract contains seaweed polyphenol and fucoxanthin, wherein the extraction rate of seaweed polyphenol can be more than 1%, such as 2% -50%, 3% -40%, 4% -20%;
for example, the seaweed extract may be prepared by a method comprising: extracting seaweed with one or more of water and organic solvent as solvent under ultrasonic condition;
the seaweed may be Ascophyllum nodosum or a mixture thereof with other seaweed.
2. The seaweed extract of claim 1, wherein the seaweed is subjected to a pretreatment prior to extraction, which may include soaking and/or crushing;
the ultrasonic extraction may be ultrasonic cell pulverization extraction, preferably, the ultrasonic extraction is performed while stirring, for example, magnetic stirring; for example, the rotation speed of the stirring is 50rpm or more, for example, 100rpm to 500rpm, 200rpm to 400 rpm;
the temperature of ultrasonic extraction may be below 60 deg.C, preferably below 50 deg.C, such as below 30 deg.C, such as below 10 deg.C;
the ultrasonic extraction time can be more than 5min, for example 10-150 min, preferably 20-90 min, such as 25-60 min and 30-45 min;
preferably, the ratio of the seaweed material to the solvent can be 1-50 g/100mL of solvent, such as 3-20 g/100mL of solvent, 6-18 g/100mL of solvent, preferably 9-15 g/100mL of solvent, more preferably 12-14 g/100mL of solvent, such as 12.81g/100mL of solvent;
the solvent can be selected from one or more of water, alcohol solvents, ester solvents and ketone solvents, preferably one or more of methanol, ethanol, propanol, isopropanol, butanol, isobutanol, ethyl acetate, methyl acetate, ethyl formate, methyl formate and acetone;
the ultrasonic power can be 95-855 w, such as 190-665 w, preferably 260-475 w;
preferably, the material obtained after extraction is further centrifuged or filtered, and the resulting supernatant or filtrate is distilled under reduced pressure and lyophilized.
3. An antibacterial agent for seaweed comprising a complex of the seaweed extract of claim 1 or 2 and an anionic surfactant;
the preparation method of the antibacterial agent comprises the following steps: mixing the seaweed extract with an anionic surfactant to obtain a seaweed-anionic surfactant complex;
the anionic surfactant may be in the form of an anionic surfactant powder or in the form of an aqueous solution;
the ratio of anionic surfactant to seaweed extract may be from 1% to 8% by volume, preferably from 2% to 5% by volume;
the anionic surfactant may be selected from one or more of sodium lauroyl sarcosinate, sodium dodecyl sulfonate, etc.;
preferably, the method further comprises mixing the seaweed extract with an anionic surfactant, standing overnight, precipitating, and removing supernatant to obtain the seaweed extract-anionic surfactant complex.
4. An algal antimicrobial composition comprising the algal antimicrobial of claim 3 and optionally one or more of a surfactant, an antioxidant, water;
preferably, the antibacterial active ingredient in the seaweed antibacterial composition is the seaweed antibacterial agent;
wherein, when one or more of the components in the seaweed antibacterial composition exist, the mixture ratio of the components can be as follows:
more than 0.1 weight part of seaweed antibacterial agent;
1 to 60 parts by weight of a surfactant;
0.05 to 10 parts by weight of antioxidant;
20 to 100 parts by weight of water;
wherein the seaweed antibacterial agent is preferably 0.5 to 50 parts by weight, such as 1 to 5 parts by weight;
the surfactant may be 1 to 60 parts by weight, preferably 5 to 50 parts by weight, for example 8 to 25 parts by weight;
the antioxidant may be 0.05 to 10 parts by weight, preferably 0.1 to 5 parts by weight, for example 0.2 to 1 part by weight;
the water may be 20 to 100 parts by weight, preferably 30 to 95 parts by weight, for example 50 to 90 parts by weight.
5. An algal antibacterial composition according to claim 4, wherein the antioxidant is independently selected from ascorbic acid and its sodium salt, erythorbic acid and its sodium salt, natural products phytic acid i.e. phytic acid, Butyl Hydroxyanisole (BHA), dibutyl hydroxytoluene (BHT) and Propyl Gallate (PG), ethoxyquin, mixed tocopherol concentrate and guaiac resin, lipoic acid, 2, 6-di-tert-butylcresol, ascorbyl palmitate, lauryl thiodipropionate, lecithin, metabisulfite, ascorbyl stearate, amyl gallate, vanillylamide, carnosol, rosmanol, epigallocatechin gallate, epicatechin gallate, catechin, astaxanthin, vitamins, citric acid, carotene, carotenoid or a combination of two or more thereof;
the surfactant may be a nonionic surfactant and/or an amphoteric surfactant, and when a mixture of nonionic and amphoteric surfactants is used, the weight ratio of the nonionic to amphoteric surfactants may be 10:1 to 1:10, such as 10:1 to 1.5:1, e.g., 5:2, 4:3, 2: 1; wherein it is preferred that, among others,
the nonionic surfactant is independently selected from sorbitan ester, sucrose ester, alkyl glycoside or combination of two or more thereof;
the amphoteric surfactant is independently selected from amino acid surfactant, betaine amphoteric surfactant or their combination;
preferably, the amino acid surfactant is an alkyl aminopropionate, a hydrochloride of an alkyl aminopropionate, more preferably a dodecyl aminopropionate, a hydrochloride of a dodecyl aminopropionate;
the water is purified water.
6. The algal antibacterial composition of claim 4 or 5, wherein the pH of the algal antibacterial composition may be 4.5 to 6.5, preferably 5.0 to 5.9;
the pH value of the seaweed antibacterial composition can be adjusted by an antioxidant or by adding an additional pH adjusting agent; the additional pH modifier may be selected from one or more of citric acid, malic acid, tartaric acid, lactic acid, acetic acid, phosphoric acid.
7. A process for the preparation of the algal antibacterial composition according to any one of claims 4-6, comprising mixing the required components of the algal antibacterial composition;
for example, the preparation method comprises the following steps:
1) mixing the seaweed antibacterial agent with water;
2) mixing a nonionic surfactant with the mixture obtained in step 1);
3) adding an amphoteric surfactant into the mixture obtained in the step 2) and mixing;
4) mixing an antioxidant with the mixture obtained in the step 3) to obtain the seaweed antibacterial composition.
8. The method of claim 7, further comprising agitating the mixture in one or more steps;
the temperature of the one or more steps may be below 50 ℃, for example below 40 ℃;
preferably, the preparation method further comprises controlling the temperature of one or more steps;
preferably, the preparation method further comprises the steps of cooling and defoaming after the components required by the seaweed antibacterial composition are mixed, so as to obtain the seaweed antibacterial composition.
9. A kit comprising the algal antimicrobial composition of any one of claims 4-6, wherein the algal antimicrobial composition within the kit is contacted with an inert atmosphere; preferably, the seaweed antibacterial composition in the kit is in an inert atmosphere.
10. A cleaning agent comprising the algal antibacterial composition of any one of claims 4-6; preferably, the cleaning agent may be selected from the group consisting of tableware, skin, fruit and vegetable, laundry detergents; preferably baby or child bottle or bottle detergents; skin detergent for infant or children such as hand cleanser and face cleanser.
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CN105996027A (en) * 2016-05-07 2016-10-12 集美大学 Functional food with effects of protecting liver and improving eyesight
CN105996027B (en) * 2016-05-07 2019-05-10 集美大学 A kind of functional food of liver protection and eyesight
CN107761354A (en) * 2017-09-21 2018-03-06 无锡德冠生物科技有限公司 One kind neutralizes sour agent and preparation method thereof
CN109673638A (en) * 2019-01-24 2019-04-26 大连大学 A kind of efficient mobile phone thimerosal
CN109706001A (en) * 2019-01-31 2019-05-03 东莞市立顿洗涤用品实业有限公司 Prevent flat bottle cleaning toilet essence and preparation method thereof
CN111068633A (en) * 2020-01-31 2020-04-28 广州绿邦环境技术有限公司 Organic water purifying agent and production process thereof
CN111529522A (en) * 2020-06-29 2020-08-14 苏州大学 Application of EGCG in preparation of preparation or food for preventing pathogenic bacterial infection
CN112646668A (en) * 2020-12-01 2021-04-13 建昌帮药业有限公司 Wool product detergent and preparation method thereof
CN112646668B (en) * 2020-12-01 2021-10-08 建昌帮药业有限公司 Wool product detergent and preparation method thereof
CN115553303A (en) * 2021-11-24 2023-01-03 吴杨 Degerming deodorant and preparation method thereof
CN114907916A (en) * 2022-04-27 2022-08-16 创灵科研发展有限公司 Metal ion bismuth combined functional antibacterial washing solution

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