CN109329702B - Compound bactericide of plant extract and preparation method thereof - Google Patents
Compound bactericide of plant extract and preparation method thereof Download PDFInfo
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- CN109329702B CN109329702B CN201811450071.6A CN201811450071A CN109329702B CN 109329702 B CN109329702 B CN 109329702B CN 201811450071 A CN201811450071 A CN 201811450071A CN 109329702 B CN109329702 B CN 109329702B
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 36
- 239000000419 plant extract Substances 0.000 title claims abstract description 36
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000003899 bactericide agent Substances 0.000 title claims abstract description 12
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- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims abstract description 56
- 241000894006 Bacteria Species 0.000 claims abstract description 33
- 239000000284 extract Substances 0.000 claims abstract description 29
- 235000014655 lactic acid Nutrition 0.000 claims abstract description 28
- 239000004310 lactic acid Substances 0.000 claims abstract description 28
- 240000002234 Allium sativum Species 0.000 claims abstract description 27
- 235000004611 garlic Nutrition 0.000 claims abstract description 27
- 235000016639 Syzygium aromaticum Nutrition 0.000 claims abstract description 26
- 244000223014 Syzygium aromaticum Species 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 244000024873 Mentha crispa Species 0.000 claims abstract description 24
- 235000014749 Mentha crispa Nutrition 0.000 claims abstract description 24
- HIQIXEFWDLTDED-UHFFFAOYSA-N 4-hydroxy-1-piperidin-4-ylpyrrolidin-2-one Chemical compound O=C1CC(O)CN1C1CCNCC1 HIQIXEFWDLTDED-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012153 distilled water Substances 0.000 claims abstract description 21
- 235000007265 Myrrhis odorata Nutrition 0.000 claims abstract description 15
- 240000004760 Pimpinella anisum Species 0.000 claims abstract description 15
- 235000012550 Pimpinella anisum Nutrition 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims description 26
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- 238000002156 mixing Methods 0.000 claims description 4
- 239000001683 mentha spicata herb oil Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 235000019721 spearmint oil Nutrition 0.000 claims description 2
- 244000063299 Bacillus subtilis Species 0.000 abstract description 9
- 235000014469 Bacillus subtilis Nutrition 0.000 abstract description 9
- 241000588724 Escherichia coli Species 0.000 abstract description 8
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 8
- 241000193830 Bacillus <bacterium> Species 0.000 abstract description 6
- 239000003242 anti bacterial agent Substances 0.000 abstract description 6
- 208000001848 dysentery Diseases 0.000 abstract description 6
- 241000222122 Candida albicans Species 0.000 abstract description 2
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- 230000001580 bacterial effect Effects 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
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- 238000000605 extraction Methods 0.000 description 2
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- 244000005700 microbiome Species 0.000 description 2
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- 231100000331 toxic Toxicity 0.000 description 2
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- FJKROLUGYXJWQN-UHFFFAOYSA-M 4-hydroxybenzoate Chemical compound OC1=CC=C(C([O-])=O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-M 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
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- 238000004945 emulsification Methods 0.000 description 1
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 1
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- 235000019249 food preservative Nutrition 0.000 description 1
- 239000005452 food preservative Substances 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
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- 230000002335 preservative effect Effects 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 229940007046 shigella dysenteriae Drugs 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 235000010199 sorbic acid Nutrition 0.000 description 1
- 239000004334 sorbic acid Substances 0.000 description 1
- 229940075582 sorbic acid Drugs 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000008223 sterile water Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3481—Organic compounds containing oxygen
- A23L3/3508—Organic compounds containing oxygen containing carboxyl groups
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Nutrition Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Botany (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a plant extract compound bactericide which is prepared from the following components in parts by weight: 5-10 parts of anise essential oil, 5-10 parts of clove essential oil, 5-10 parts of spearmint essential oil, 5-10 parts of isopropyl myristate, 10-20 parts of garlic water extract, 0.5-1 part of lactic acid, 80-160 parts of distilled water, 5-30 parts of tween-8015, 5-30 parts of RH-4015 and 15-30 parts of absolute ethyl alcohol. The invention also discloses a preparation method of the composition. The plant extract compound antibacterial agent has obvious antibacterial and antibacterial effects on common food-borne bacteria in life, such as escherichia coli, staphylococcus aureus, bacillus subtilis, candida albicans, dysentery bacillus and the like.
Description
Technical Field
The invention relates to the technical field of food bacteriostasis, in particular to a plant extract compound bactericide and a preparation method thereof.
Background
Food products are difficult to protect from microbial contamination during storage and use. In order to prolong the shelf life of food products, various means have been used to inactivate microorganisms and retard or prevent their growth, the addition of preservatives being a convenient, effective and commonly used method. The food preservatives used at present mainly comprise chemical preservatives such as benzoic acid, sorbic acid and salts thereof, p-hydroxybenzoate and the like, and although the chemical preservatives have a certain inhibiting effect on microorganisms, most of the chemical preservatives have certain physiological toxicity, and the long-term accumulation can cause the function of a human body to be reduced, even cause serious health problems. Therefore, the research and development of natural preservatives which are convenient to use, good in effect and free of toxic and side effects are generally regarded by all countries in the world. The plant type seasoning is one of important sources of natural preservatives, the raw materials are easy to obtain and low in price, natural ingredients are not easy to generate drug resistance, efficient and economical preservative substances are screened out from the natural preservatives and used in combination with other natural bacteriostatic agents, the bacteriostatic effect can be synergistically increased, the bacteriostatic cost can be reduced, and therefore the plant type seasoning has a wide application prospect.
Most of the plant essential oil is water-insoluble, and is difficult to be directly applied to food production, the solubility of the plant essential oil is usually increased by adopting an emulsification mode, but the conventional emulsion has large particle size and poor actual use effect, and is easy to have unfavorable phenomena such as demulsification, oxidation and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a plant extract compound bacteria reducing agent and a preparation method thereof.
In order to solve the technical problems, the invention provides a plant extract compound bactericide which is prepared from the following components in parts by weight: 5-10 parts of anise essential oil, 5-10 parts of clove essential oil, 5-10 parts of spearmint essential oil, 5-10 parts of isopropyl myristate, 10-20 parts of garlic water extract, 0.5-1 part of lactic acid, 80-160 parts of distilled water, 5-30 parts of tween-8015, 15-30 parts of RH-40 (polyoxyethylene-40 hydrogenated castor oil) and 15-30 parts of absolute ethyl alcohol.
The improvement of the plant extract compound bacteria reducing agent of the invention is as follows:
anise essential oil: clove essential oil: spearmint essential oil: isopropyl myristate: garlic water extract: lactic acid 10: 10: 10: 10: 20: 1, mass ratio.
The plant extract compound bacteria reducing agent is further improved as follows:
tween-80: RH-40: anhydrous ethanol ═ 1: 1: 1, mass ratio.
The plant extract compound bacteria reducing agent is further improved as follows: the composition comprises the following components in parts by weight: 8 parts of star anise essential oil, 8 parts of clove essential oil, 8 parts of spearmint oil, 8 parts of isopropyl myristate, 16 parts of garlic water extract, 0.8 part of lactic acid, 140 parts of distilled water, 25 parts of tween-8025 parts, 5 parts of RH-4025 parts and 25 parts of absolute ethyl alcohol.
The invention also provides a preparation method of the plant extract compound bacteria reducing agent, which comprises the following steps:
1) mixing the anise essential oil, the clove essential oil and the spearmint essential oil, and then ultrasonically dissolving the mixture in isopropyl myristate to obtain an oil phase;
2) dissolving the garlic water extract and lactic acid in distilled water to obtain a water phase;
3) sequentially adding absolute ethyl alcohol (slowly adding for about 1-2 minutes), tween-80 and RH-40 into the oil phase, and performing high-speed shearing treatment to obtain a mixture;
note: absolute ethyl alcohol is taken as an auxiliary emulsifier, and Tween-80 and RH-40 are taken as emulsifiers;
4) dropwise adding (the dropwise adding time is 3-5 minutes) a water phase into the mixture, and performing high-speed shearing treatment to obtain an emulsion;
5) and carrying out high-pressure homogenization treatment on the emulsion by using a high-pressure homogenizer to obtain the plant extract compound bacteria reducing agent (called compound bacteria reducing agent for short).
The improvement of the preparation method of the plant extract compound bacteria reducing agent of the invention comprises the following steps:
the high-speed shearing treatment of the step 3): shearing at 6000-8000 r/min for 40-60 s (which can be performed in a high-shear dispersion emulsifier),
the high-speed shearing treatment in the step 4): high-shearing treatment is carried out for 60-80 s at 8000-10000 r/min (which can be carried out in a high-shearing dispersion emulsifying machine),
in the step 5), the operation pressure is 60 MPa-65 MPa, and the high-pressure homogenization treatment is circulated for 4-6 times (each treatment time is about 5-10 minutes), so that the nano emulsion (the nano emulsion with the average particle size of less than 100 nm) is obtained, wherein the nano emulsion is a plant extract compound bactericide.
The bacteria reducing agent is prepared by compounding natural plant extracts, natural lactic acid and an emulsifier/co-emulsifier and performing high-shear action and high-pressure homogenization treatment, has an obvious bacteria reducing effect on common bacteria, has a lasting effect, and also has the advantages of simple preparation method and low cost.
Compared with the prior art, the plant extract compound bacteria reducing agent and the preparation method thereof have the following technical advantages:
1) the extracts of edible natural plants are taken as main bacteriostatic components, and the extracts mainly comprise anise essential oil, clove essential oil, spearmint essential oil and garlic aqueous extract, so that the extraction method is green and environment-friendly, the extracts are safe in components, small in toxic and side effects on a human body, and not easy to generate drug resistance, and raw materials are easy to obtain, the extraction method is simple, and the processing cost is low;
2) lactic acid is a natural bacteriostatic substance, has a good bacteriostatic effect, but is not widely applied, and is easy to change the sensory quality of food due to the fact that high concentration is needed when the lactic acid is used alone, so that the lactic acid has poor taste and flavor and is high in price; the screened plant type extract with better bacteria reduction effect is optimally compounded with natural lactic acid, and can play a role in synergy under the condition of using a very small amount of lactic acid, so that the range of a bacteriostatic spectrum is expanded, and the production cost is further reduced;
3) compared with the conventional emulsion, the nano-emulsion can construct an optically transparent system, increase the bioavailability of the effective substances, improve the stability of the effective substances, play a certain slow-release effect and have far-reaching significance in the research and development of foods.
The invention adopts high-shear and high-pressure homogenization treatment technology, reduces the average grain size of the bacteriostatic agent to the nanometer level by optimizing the proportion of the oil phase, the water phase, the emulsifier and the co-emulsifier and the treatment conditions, has uniform grain size and good stability, can obviously improve the bacteriostatic effect of bacteriostatic components and prolong the duration of the bacteriostatic effect.
4) Experiments prove that: the plant extract compound antibacterial agent provided by the invention has obvious antibacterial and antibacterial effects on common food-borne bacteria in life, such as escherichia coli, staphylococcus aureus, bacillus subtilis, candida albicans, dysentery bacillus and the like, and compared with a non-nanoemulsion antibacterial agent, a nanoemulsion antibacterial agent has more stable effect and longer duration.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
in the invention, the anise essential oil, the clove essential oil, the spearmint essential oil and the garlic water extract can be prepared according to the conventional method,
the preparation method of the anise essential oil comprises the following steps: taking dried star anise (the water content is less than or equal to 5 percent), crushing, sieving with a 40-mesh sieve, weighing 10 parts by weight of dried powder, putting the dried powder into a filter paper bag, adding 100 parts by weight of absolute ethyl alcohol (namely, the material-liquid ratio is 10g/100ml), heating in a water bath at 70 ℃, circularly leaching until the color of a new leaching solution is not changed, taking out the leaching solution, removing the absolute ethyl alcohol by reduced pressure distillation, and adding a small amount of anhydrous sodium sulfate for dehydration to obtain the star anise essential oil.
The star anise is changed into clove and spearmint, and the clove essential oil and the spearmint essential oil can be correspondingly obtained by preparing according to the method.
The preparation method of the garlic aqueous extract comprises the following steps: weighing fresh garlic 10 parts by weight, adding sterile distilled water 10 parts by weight, crushing with a wall breaking machine for 5min, taking out, homogenizing at 15000r/min for 5min, transferring into a centrifuge tube, centrifuging at 8000r/min for 15min, and collecting supernatant to obtain garlic water extract.
Examples 1,
A compound bactericide of plant extracts comprises the following raw materials in percentage by mass: 5 parts of anise essential oil, 5 parts of clove essential oil, 5 parts of spearmint essential oil, 5 parts of isopropyl myristate, 10 parts of garlic water extract, 0.5 part of lactic acid, 100 parts of distilled water, 5 parts of tween-8015 parts of RH-4015 parts and 15 parts of absolute ethyl alcohol.
The preparation method comprises the following steps in sequence:
s1, accurately weighing the anise essential oil, the clove essential oil and the spearmint essential oil, mixing, and performing ultrasonic treatment at 30kHz for 10min to fully dissolve the essential oil in isopropyl myristate to obtain an oil phase;
s2, accurately weighing garlic water extract and lactic acid, and dissolving in distilled water to obtain water phase;
s3, slowly adding (adding for about 2 minutes) co-emulsifier absolute ethyl alcohol into the oil phase, adding emulsifiers Tween-80 and RH-40, and performing high-shear treatment for 40S at 6000r/min by using a high-shear dispersion emulsifying machine to obtain a mixture;
s4, dropwise adding a water phase into the mixture (the dropwise adding time is about 5 minutes), and performing high-shear treatment for 60S at 8000r/min by using a high-shear dispersion emulsifier to obtain an emulsion;
and S5, carrying out high-pressure homogenization treatment on the emulsion by using a high-pressure homogenizer, wherein the operation pressure is 60MPa, and the high-pressure homogenization treatment is circulated for 4 times (each treatment time is about 8 minutes) to obtain the nano emulsion which is the plant extract compound bacteria reducing agent.
Embodiment 2, a plant extract compound bacteria reducing agent comprises the following raw materials in parts by mass: 6 parts of anise essential oil, 6 parts of clove essential oil, 6 parts of spearmint essential oil, 6 parts of isopropyl myristate, 12 parts of garlic water extract, 0.6 part of lactic acid, 100 parts of distilled water, 5 parts of tween-8015 parts of RH-4015 parts and 15 parts of absolute ethyl alcohol.
The preparation method is identical to example 1.
Embodiment 3, a plant extract compound bacteria reducing agent comprises the following raw materials in parts by mass: 8 parts of star anise essential oil, 8 parts of clove essential oil, 8 parts of spearmint essential oil, 8 parts of isopropyl myristate, 16 parts of garlic water extract, 0.8 part of lactic acid, 100 parts of distilled water, 5 parts of tween-8015 parts of RH-4015 parts and 15 parts of absolute ethyl alcohol.
The preparation method is identical to example 1.
Embodiment 4, a plant extract compound bacteria reducing agent comprises the following raw materials in parts by mass: 10 parts of anise essential oil, 10 parts of clove essential oil, 10 parts of spearmint essential oil, 10 parts of isopropyl myristate, 20 parts of garlic water extract, 1.0 part of lactic acid, 100 parts of distilled water, 5 parts of tween-8015 parts of RH-4015 parts and 15 parts of absolute ethyl alcohol.
The preparation method is identical to example 1.
Embodiment 5, a plant extract compound bacteria reducing agent comprises the following raw materials in parts by mass: 8 parts of star anise essential oil, 8 parts of clove essential oil, 8 parts of spearmint essential oil, 8 parts of isopropyl myristate, 16 parts of garlic water extract, 0.8 part of lactic acid, 120 parts of distilled water, 20 parts of tween-8020 parts, RH-4020 parts and 20 parts of absolute ethyl alcohol.
The preparation method is identical to example 1.
Embodiment 6, a plant extract compound bacteria reducing agent comprises the following raw materials in parts by mass: 8 parts of star anise essential oil, 8 parts of clove essential oil, 8 parts of spearmint essential oil, 8 parts of isopropyl myristate, 16 parts of garlic water extract, 0.8 part of lactic acid, 140 parts of distilled water, 25 parts of tween-8025 parts, 5 parts of RH-4025 parts and 25 parts of absolute ethyl alcohol.
The preparation method is identical to example 1.
Embodiment 7, a plant extract compound bacteria reducing agent comprises the following raw materials in parts by mass: 8 parts of star anise essential oil, 8 parts of clove essential oil, 8 parts of spearmint essential oil, 8 parts of isopropyl myristate, 16 parts of garlic water extract, 0.8 part of lactic acid, 140 parts of distilled water, 25 parts of tween-8025 parts, 5 parts of RH-4025 parts and 25 parts of absolute ethyl alcohol.
The preparation method, S3, is changed into 'high shear treatment for 60S at 8000 r/min', and the rest is identical to that of example 1.
The embodiment 8 discloses a plant extract compound bacteria reducing agent which comprises the following raw materials in parts by mass: 8 parts of star anise essential oil, 8 parts of clove essential oil, 8 parts of spearmint essential oil, 8 parts of isopropyl myristate, 16 parts of garlic water extract, 0.8 part of lactic acid, 140 parts of distilled water, 25 parts of tween-8025 parts, 5 parts of RH-4025 parts and 25 parts of absolute ethyl alcohol.
The preparation method was changed to "60S at 8000r/min high shear treatment" in S3 and "80S at 10000r/min high shear treatment" in S4, and the rest was the same as example 1.
Embodiment 9, a plant extract compound bacteria reducing agent comprises the following raw materials in parts by mass: 8 parts of star anise essential oil, 8 parts of clove essential oil, 8 parts of spearmint essential oil, 8 parts of isopropyl myristate, 16 parts of garlic water extract, 0.8 part of lactic acid, 140 parts of distilled water, 25 parts of tween-8025 parts, 5 parts of RH-4025 parts and 25 parts of absolute ethyl alcohol.
The preparation method comprises changing the high-shear treatment at 8000r/min to 60S in S3, changing the high-shear treatment at 10000r/min to 80S in S4, and changing the pressure to 65MPa in S5; the rest is equivalent to embodiment 1.
The embodiment 10 discloses a plant extract compound bacteria reducing agent, which comprises the following raw materials in percentage by mass: 8 parts of star anise essential oil, 8 parts of clove essential oil, 8 parts of spearmint essential oil, 8 parts of isopropyl myristate, 16 parts of garlic water extract, 0.8 part of lactic acid, 140 parts of distilled water, 25 parts of tween-8025 parts, 5 parts of RH-4025 parts and 25 parts of absolute ethyl alcohol.
The preparation method comprises changing the high-shear treatment at 8000r/min to 60S in S3, changing the high-shear treatment at 10000r/min to 80S in S4, changing the high-shear treatment at 65MPa in S5, and changing the cycle number to 6 times; the rest is equivalent to embodiment 1.
Embodiment 11, a plant extract compound bacteria reducing agent comprises the following raw materials in parts by mass: 8 parts of star anise essential oil, 8 parts of clove essential oil, 8 parts of spearmint essential oil, 8 parts of isopropyl myristate, 16 parts of garlic water extract, 0.8 part of lactic acid, 140 parts of distilled water, 25 parts of tween-8025 parts, 5 parts of RH-4025 parts and 25 parts of absolute ethyl alcohol.
The preparation method, step S5 is eliminated; the rest is equivalent to the embodiment 1; namely, the emulsion obtained in S4 was used as a microbial reducing agent.
Experiment 1, the particle size of the microbial inoculum prepared in examples 1 to 11 is measured, the average particle size of the microbial inoculum prepared in examples 1 to 11 is measured by a laser particle size analyzer and recorded, and the obtained results are as shown in table 1 below:
TABLE 1 average particle diameter of the fungicide obtained in each example
| Example numbering | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 |
| Average particle diameter/nm | 64 | 61 | 69 | 96 | 67 | 55 | 51 | 43 | 22 | 31 | 265 |
Experiment 2, sterilization test:
1. test strains:
escherichia coli, Staphylococcus aureus, Bacillus subtilis, and Bacillus dysenteriae;
2. test agents:
(1) the antibacterial agent prepared in the embodiments 1-11 of the invention;
(2) common disinfectant
3. The test method comprises the following steps:
(1) activating the tested strain, performing amplification culture in nutrient broth culture medium, and diluting according to McLeod's turbidimetry until the tested strain concentration is 107CFU/ml；
(2) Filling 4ml of nutrient broth culture medium into the test tube, plugging and sterilizing for later use;
(3) respectively adding 4ml of the bacteria-reducing agent prepared in the embodiment 1-11 of the invention into a sterilized broth test tube in a sterile environment, sequentially marking as No. 1-11, adding an equal amount of common disinfectant into a 12 th test tube, marking as No. 12, and adding 4ml of sterile water into 13 th and 14 th test tubes, marking as No. 13 and No. 14;
(4) sequentially adding 0.1ml of tested bacterial liquid into the test tube No. 1-13 prepared in the step (3), adding no bacterial liquid into the test tube No. 14, taking blank control, performing shake culture at 37 ℃ for 12-72 h after plugging, and observing turbidity of the test tube;
(5) and (3) respectively sucking 0.1ml of culture solution in the 14 test tubes in the step (4) to a sterile plate, pouring the culture solution into a plate counting culture medium, uniformly mixing, standing, inverting after coagulation, culturing at 37 ℃ for 24 hours, and counting.
4. Experimental results (bacteria-reducing effect):
1) escherichia coli
TABLE 2 inhibitory Effect of examples on Escherichia coli
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | 14 | |
| Clarity (12h) | - | - | - | - | - | - | - | - | - | - | - | - | + | - |
| Clarity (24h) | - | - | - | - | - | - | - | - | - | - | - | - | ++ | - |
| Clarity (48h) | - | - | - | - | - | - | - | - | - | - | + | + | ++ | - |
| Clarity (72h) | + | - | + | + | + | - | - | - | - | - | ++ | ++ | ++ | - |
Note: "-" represents clear, "+" represents turbid, and more "+" represents more turbid.
TABLE 3 bactericidal effect of examples on E.coli
Note: "-" represents sterility, "+" indicates sterility, but the total number of colonies counted on the plate is less than or equal to 5, and more "+" indicates more colonies.
2) Staphylococcus aureus
TABLE 4 bacteriostatic effect of examples on Staphylococcus aureus
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | 14 | |
| Clarity (12h) | - | - | - | - | - | - | - | - | - | - | - | - | ++ | - |
| Clarity (24h) | - | - | - | - | - | - | - | - | - | - | - | - | ++ | - |
| Clarity (48h) | - | - | - | - | - | - | - | - | - | - | - | + | ++ | - |
| Clarity (72h) | + | - | - | + | - | - | - | - | - | - | + | + | ++ | - |
Note: "-" represents clear, "+" represents turbid, and more "+" represents more turbid.
TABLE 5 bactericidal effect of examples on Staphylococcus aureus
Note: "-" represents sterility, "+" indicates presence of bacteria, but the total number of colonies is 5, and more "+" indicates more colonies.
3) Bacillus subtilis and bacillus subtilis
TABLE 6 bacteriostatic effect of examples on Bacillus subtilis
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | 14 | |
| Clarity (12h) | - | - | - | - | - | - | - | - | - | - | - | - | + | - |
| Clarity (24h) | - | - | - | - | - | - | - | - | - | - | - | + | ++ | - |
| Clarity (48h) | + | - | - | - | - | - | - | - | - | - | - | + | ++ | - |
| Clarity (72h) | ++ | + | - | + | - | - | - | - | - | - | + | ++ | ++ | - |
Note: "-" represents clear, "+" represents turbid, and more "+" represents more turbid.
TABLE 7 bactericidal effect of examples on Bacillus subtilis
Note: "-" represents sterility, "+" indicates presence of bacteria, but the total number of colonies is 5, and more "+" indicates more colonies.
4) Dysentery bacillus
TABLE 8 bacteriostatic effect of examples on dysentery bacillus
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | 14 | |
| Clarity (12h) | - | - | - | - | - | - | - | - | - | - | - | - | + | - |
| Clarity (24h) | - | - | - | - | - | - | - | - | - | - | - | - | ++ | - |
| Clarity (48h) | - | - | - | - | - | - | - | - | - | - | - | + | ++ | - |
| Clarity (72h) | + | + | - | - | + | - | - | - | - | - | + | ++ | ++ | - |
Note: "-" represents clear, "+" represents turbid, and more "+" represents more turbid.
TABLE 9 sterilizing effect of examples on dysentery bacillus
Note: "-" represents sterility, "+" indicates presence of bacteria, but the total number of colonies is 5, and more "+" indicates more colonies.
By analyzing and comparing the data of the various examples, the proportion of the components such as the extract, the emulsifier, the distilled water and the like and the process conditions of high-shear treatment and high-pressure homogenization treatment have significant influence on the average particle size of the bactericide nano-emulsion.
1. By comparing the results of examples 1 to 6 (these 6 cases, only formulation differences) it can be found that:
the proportion relationship of the oil phase (anise essential oil, clove essential oil, spearmint essential oil and isopropyl myristate), the main components (garlic water extract and lactic acid) and the auxiliary/emulsifier in the water phase is very important: the content of the main components in the oil phase and the water phase of example 6 (best case) is lower than that of examples 2, 3, 4 and 5; but the final bacteriostatic/bactericidal effect was superior to examples 2, 3, 4, 5.
2. By comparing the results of examples 6 to 11 (these 6 cases, the formula is the same, and the process is slightly different), it can be found that:
in examples 6 to 10, the formed average particle size was 22 to 55nm, and thus the bacteriostatic/bactericidal effects obtained were substantially the same, whereas in example 11, the obtained average particle size was 265nm, which is far inferior to those in examples 6 to 10. Thus: the smaller the particle size of the nano-emulsion is, the more stable the emulsion system is relatively, and the longer the bactericidal effect of the bacteriostatic agent is.
By analyzing the experimental data of tables 1 to 9, it was found that: the prepared antibacterial agent has good antibacterial and bactericidal effects on escherichia coli, staphylococcus aureus, bacillus subtilis and shigella dysenteriae, and the action time is long; and the bacteriostatic and bactericidal effects and the duration of action on the common bacteria are superior to those of common disinfectant.
Comparative examples 1 to 6, the formulation was changed as described in table 10 below, and the preparation method was identical to example 6.
Watch 10
The bacteriostatic/bactericidal effects of comparative examples 1 to 6 above were compared with those of example 6, as shown in table 11 below.
TABLE 11 colony count (72h)
| Escherichia coli | Staphylococcus aureus | Bacillus subtilis | Dysentery bacillus | |
| Example 6 | + | - | - | - |
| Comparative example 1 | ++ | - | + | + |
| Comparative example 2 | ++ | + | + | - |
| Comparative example 3 | ++ | + | + | - |
| Comparative example 4 | ++ | + | + | + |
| Comparative example 5 | ++ | - | + | ++ |
| Comparative example 6 | + | + | ++ | - |
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and those skilled in the art can make modifications or equivalent substitutions on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered by the claims of the present invention.
Claims (4)
1. The compound bactericide of the plant extract is characterized by comprising the following components in parts by weight: 5-10 parts of anise essential oil, 5-10 parts of clove essential oil, 5-10 parts of spearmint essential oil, 5-10 parts of isopropyl myristate, 10-20 parts of garlic water extract, 0.5-1 part of lactic acid, 80-160 parts of distilled water, 5-30 parts of tween-8015, 5-30 parts of RH-4015 and 15-30 parts of absolute ethyl alcohol;
anise essential oil: clove essential oil: spearmint essential oil: isopropyl myristate: garlic water extract: lactic acid = 10: 10: 10: 10: 20: 1 in mass ratio;
the preparation method of the plant extract compound bacteria reducing agent comprises the following steps:
1) mixing the anise essential oil, the clove essential oil and the spearmint essential oil, and then ultrasonically dissolving the mixture in isopropyl myristate to obtain an oil phase;
2) dissolving the garlic water extract and lactic acid in distilled water to obtain a water phase;
3) sequentially adding absolute ethyl alcohol, tween-80 and RH-40 into the oil phase, and performing high-speed shearing treatment to obtain a mixture;
4) dropwise adding a water phase into the mixture, and performing high-speed shearing treatment to obtain an emulsion;
5) and carrying out high-pressure homogenization treatment on the emulsion by adopting a high-pressure homogenizer to obtain the plant extract compound bacteria reducing agent.
2. The plant extract compound bactericide as claimed in claim 1, which is characterized in that:
tween-80: RH-40: absolute ethanol = 1: 1: 1, mass ratio.
3. The plant extract compound bactericide as claimed in claim 1 or 2, which is characterized by comprising the following components in parts by weight: 8 parts of star anise essential oil, 8 parts of clove essential oil, 8 parts of spearmint oil, 8 parts of isopropyl myristate, 16 parts of garlic water extract, 0.8 part of lactic acid, 140 parts of distilled water, 25 parts of tween-8025 parts, 5 parts of RH-4025 parts and 25 parts of absolute ethyl alcohol.
4. The plant extract compound bactericide as claimed in claim 3, which is characterized in that:
the high-speed shearing treatment of the step 3): shearing at 6000-8000 r/min for 40-60 s,
the high-speed shearing treatment in the step 4): high-shear processing at 8000-10000 r/min for 60-80 s,
in the step 5), the operation pressure is 60 MPa-65 MPa, and the high-pressure homogenization treatment is circulated for 4-6 times, so that the nano emulsion is obtained, and the nano emulsion is a plant extract compound bacteria reducing agent.
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