A hot pepper extract emulsion, its preparation method and application
By preparing a stable chili extract emulsion, the problem of insufficient stability of capsaicin in the field of pesticide application was solved, achieving a highly efficient control effect on red mite pests, and is suitable for biological pesticide insecticides.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-29
- Publication Date
- 2026-03-31
AI Technical Summary
In the current technology, capsaicin has not yet formed a stable emulsion form in the field of pesticides, which makes its effect in pest control not long-lasting and stable.
A stable chili extract emulsion was prepared by using a specific ratio of wintergreen oil, ethylene glycol, defoamer, and emulsifier EL-40:S-20 through ultrasonic extraction and high-speed shear emulsification processes. This emulsion is used to prepare a biopesticide insecticide.
The prepared chili extract emulsion showed a highly effective killing effect on red mites in the control of traditional Chinese medicine, with a long duration of action and good stability under different temperature conditions, meeting relevant standards.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of biopesticide technology, specifically relating to a chili pepper extract emulsion, its preparation method, and its application. Background Technology
[0002] Chili pepper (Capsicum annuum) (Linn) is an annual or short-lived perennial herbaceous plant belonging to the genus Capsicum in the Solanaceae family. The fruit is typically conical or oblong, green when immature, turning bright red, green, or purple when ripe, with red being the most common. The fruit's spiciness comes from capsaicin in its pericarp, which enhances appetite.
[0003] Wang Xinyu et al. are the producers of capsaicin, the source of spiciness. [1] This study compared the extraction rates of capsaicin using the conventional immersion method and the ultrasonic extraction method. The ultrasonic extraction method was found to be faster and yielded a higher extraction rate than the conventional immersion method. Chili peppers can be used as a natural food additive in our daily lives. [6] It can be used for anesthesia.
[16] Anti-inflammatory and analgesic
[17] Medical fields [2] It is also commonly used in the beauty industry, including weight loss and cosmetic procedures. [7-10] In the feed industry, the application of capsaicin, with the deepening research on capsaicin in chili peppers, has revealed its antibacterial, antitoxic, and immune-enhancing properties, which can reduce the use of antibiotics.
[13] Because it does not kill marine life, capsaicin can be used in navigation as a repellent to prevent marine organisms from attaching to the hull, thus extending the hull's lifespan and reducing drag during navigation. [3] Capsicum red pigment, as a natural red pigment, not only has a bright and stable color, but also has good preservative properties.
[11] .
[0004] Gao Yan et al. [4] This study presents research on the application of capsaicin in chili peppers. Capsaicin exhibits a significant contact toxicity against pests, causing paralysis, paralysis, and ultimately death upon contact with it. Capsaicin also acts as a stomach poison, inhibiting detoxification enzymes, affecting digestion and absorption, interfering with respiratory metabolism, and hindering normal physiological activities, leading to physiological disorders, inhibited growth and development, and ultimately death.
[18] Wang Yinmin [1] They proposed formulations for green pesticides, providing theoretical guidance and applicable formulations for the use of capsaicin. (Based on Zhang Guisen)
[12] This study aims to learn about the methods and approaches to emulsion preparation, providing insights and ideas for understanding the emulsion preparation process. (Pei Chen et al.) [5]The study explored the greening agents for pesticides and their preparation mechanisms, which greatly helped provide the process and method for preparing emulsions in this invention.
[0005] Capsaicin is a natural compound produced by chili peppers and can be used as a green pesticide that is environmentally friendly and pollution-free.
[14] Chen Quling et al. found through research that rodent repellents with capsaicin as the main active ingredient have a good repellent effect on stored grain in rural areas. Repellents containing 1% capsaicin maintain their rodent-repelling effect for more than 5 months. Facing the problem of rodent infestation in rural areas, using capsaicin to make repellents can repel rodents and ants without causing pesticide contamination to grain or harm to humans, thus solving a major problem in rural grain storage. Based on the fact that capsaicin can be used as a rodent repellent in stored grain, it can be applied to agricultural production for pest control, becoming a new type of green pesticide with no residue and no harm. (Lai Guxian)
[15] Initial formulations of capsaicin as a green insect repellent showed good repellent effects on ants in experiments. Based on this approach, capsaicin could be prepared into a commonly used pesticide formulation, with a very promising future application. Summary of the Invention
[0006] The purpose of this invention is to provide a stable chili extract emulsion, its preparation method, and its application.
[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows:
[0008] The chili extract emulsion of the present invention comprises the following raw materials by mass percentage: 6-10% wintergreen oil, 2-5% ethylene glycol, 0.1-0.3% defoamer, 8-12% emulsifier, 1-3% chili extract diluent, and the balance being water.
[0009] Preferably, the chili extract emulsion of the present invention comprises the following raw materials by mass percentage: 7-9% wintergreen oil, 2-3% ethylene glycol, 0.1-0.2% defoamer, 9-11% emulsifier, 1-2% chili extract diluent, and the balance being water.
[0010] More preferably, the chili extract emulsion of the present invention comprises the following raw materials by mass percentage: 8% wintergreen oil, 2% ethylene glycol, 0.1% defoamer, 10% emulsifier, 2% chili extract diluent, and the balance being water.
[0011] The emulsifier described in this invention is EL-40:S-20 = 9:1.
[0012] The method for preparing the chili extract emulsion of the present invention includes the following steps:
[0013] (1) Preparation of dried chili powder: Remove the stems and seeds of dried red chilies, place them in a constant temperature drying oven at 50-60℃ and dry for 1.5-2.5h, pulverize them through a 40-mesh sieve, collect the dried chili powder and set aside.
[0014] (2) Chili extraction: Weigh a certain amount of chili powder, add ethanol solution at a material-to-liquid ratio of 1:4, extract by ultrasonication, filter under normal pressure, add the same volume of ethanol solution again, extract by ultrasonication under the same conditions, filter, combine the filtrates, and collect for later use.
[0015] (3) Preparation of chili extract: Collect the filtrate, concentrate it under reduced pressure, manually adjust the water bath temperature to 40-65℃, and control the rotation speed to 60-90r / min. When the filtrate evaporates to 10mL, collect the filtrate and dry it in a constant temperature oven at 120℃ to constant weight to obtain crude chili extract.
[0016] (4) Preparation of chili extract dilution: Take the crude chili extract, add 48.5 mL of wintergreen oil, sonicate to dissolve, and make up to 50 mL to prepare a chili extract dilution with a concentration of 0.03 g / mL for later use. Shake well before each use.
[0017] (5) Preparation of emulsion:
[0018] Mix the diluted chili extract with wintergreen oil according to the formula ratio, then add an emulsifier as the oil phase and deionized water as the aqueous phase. Add ethylene glycol and defoamer to the aqueous phase, and slowly pour the aqueous phase into the oil phase while stirring. Stir to form a coarse emulsion, and then use a high-speed shear emulsifier to gradually increase the speed to 8000-9000 r / min for 5 minutes to obtain a stable chili extract emulsion.
[0019] Preferably, the preparation method of the chili extract emulsion of the present invention includes the following steps:
[0020] (1) Preparation of dried chili powder: Remove the stems and seeds of dried red chilies, place them in a 50℃ constant temperature drying oven to dry for 2 hours, pulverize them through a 40-mesh sieve, collect the dried chili powder, and set aside for later use.
[0021] (2) Chili extraction: Weigh a certain amount of chili powder, add ethanol solution at a material-to-liquid ratio of 1:4, extract by ultrasonication, filter under normal pressure, add the same volume of ethanol solution again, extract by ultrasonication under the same conditions, filter, combine the filtrates, and collect for later use.
[0022] (3) Preparation of chili extract: The collected filtrate was concentrated under reduced pressure. The water bath temperature was manually adjusted to 40℃ and the rotation speed was controlled at 60r / min. When the filtrate evaporated to 10mL, the filtrate was collected and dried in a constant temperature oven at 120℃ to constant weight to obtain crude chili extract.
[0023] (4) Preparation of chili extract dilution: Take the crude chili extract, add 48.5 mL of wintergreen oil, dissolve by sonication, and make up the volume of the chili extract and wintergreen oil mixture to 50 mL to prepare a chili extract dilution with a concentration of 0.03 g / mL for later use. Shake well before each use.
[0024] (5) Preparation of emulsion:
[0025] The diluted chili extract and wintergreen oil were mixed according to the formula ratio. Then, an emulsifier was added as the oil phase and deionized water as the aqueous phase. Ethylene glycol and defoamer were added to the aqueous phase. The aqueous phase was slowly poured into the oil phase while stirring. The mixture was stirred to form a crude emulsion. Then, a high-speed shear emulsifier was used to gradually increase the speed to 9000 r / min for 5 minutes to obtain a stable chili extract emulsion.
[0026] The ethanol solution mentioned in step (2) of this invention is 95% ethanol.
[0027] The ultrasonic extraction conditions described in step (2) of this invention are: ultrasonic extraction for 30-40 min, with a power of 80-100 W.
[0028] Preferably, the ultrasonic extraction conditions in step (2) of the present invention are: ultrasonication for 35 minutes and power of 90W.
[0029] The application of the chili extract emulsion described in this invention or the chili extract emulsion prepared by the method described herein in the preparation of biological pesticides for preventing or killing red mites that are pests of Chinese medicinal herbs.
[0030] Beneficial effects:
[0031] 1. This invention measures the stability, dispersibility, thermal storage stability, and cold storage stability of the emulsion, and conducts screening experiments on the dosage of ethylene glycol and defoamer. A suitable emulsion formulation was ultimately selected: 8% wintergreen oil, 2% ethylene glycol, 0.1% defoamer, 10% EL-40:S-20 (9:1) emulsifier, 2 mL of chili extract (diluted chili extract solution), and ultrapure water to a final volume of 100 mL. Analysis using a zeta potential and nanoparticle size analyzer showed that the emulsion prepared at 9000 r / min exhibited a good particle size distribution curve with a δ value of 1.48. Furthermore, the product meets the relevant national standards.
[0032] 2. This invention conducted screening experiments to investigate the selection of emulsifiers. The results showed that By140, EL-40, 2301, 500#, and S-20 all had emulsifying effects. However, By140, 2301, and 500# emulsifiers failed the tests for stability in both hot and cold storage. 601 did not have an emulsifying effect, so no cold or hot storage tests were conducted. By selecting S-20 and EL-40 for compounding experiments, the results showed that the emulsion tended to be more stable as the amount of EL-40 increased. Therefore, the preferred emulsifier ratio was 9:1 (EL-40:S-20).
[0033] 3. This invention conducted screening experiments on the dosage of ethylene glycol and defoamer. The results showed that: in the freeze-thaw experiment without adding ethylene glycol, the amount of oil separation decreased after adding ethylene glycol, and the optimal dosage of ethylene glycol was 2%. Without adding defoamer, a large number of bubbles were generated during the emulsifier preparation shearing process, and they dissipated slowly, increasing the volume of the emulsion and affecting subsequent experimental observation and judgment. After adding an organosilicon defoamer, the bubbles dissipated quickly and without large or small bubbles, and the optimal dosage of defoamer was 0.1%.
[0034] 4. In the thermal storage stability test, it was found that as the rotation speed increases, the emulsifier can be better emulsified with the oil phase and uniformly dispersed in the aqueous phase. When the rotation speed is between 5000-7000 r, there is oil separation to varying degrees. When the rotation speed reaches 8000 r, no oil phase is separated. At 9000 r, the particle size range is small and the emulsion is more stable. Therefore, the preferred rotation speed is 9000 r.
[0035] 5. The preparation method of this invention is simple and easy to implement. The prepared chili extract emulsion is stable. The results of the emulsion performance evaluation are as follows: After diluting the emulsion sample 200 times in standard hard water and allowing it to stand for 1 hour, no floating oil, no sediment, and no stratification were observed, indicating that the emulsion stability was qualified. However, the emulsion dispersibility was good; some particles settled but were basically dispersed, which was considered good. For heat storage stability testing, a small amount of oil separation was observed, but after gentle shaking and thorough mixing, the emulsion's heat storage stability was qualified. For low-temperature stability testing, after being placed in a refrigerator at (0±2)℃ for 7 days, no oil separation was observed, and the centrifugal precipitate did not exceed 0.3%, indicating that the emulsion's low-temperature stability was qualified.
[0036] 6. The chili extract emulsion prepared by this invention, when diluted 100 times, has a single-use red mite killing effect of over 85%, and after 7 days of use, the repellency and killing rate can reach over 90%; it also has a long-lasting effect and a good control effect on red mite pests in traditional Chinese medicine. Attached Figure Description
[0037] Figure 1 Graphs of analytical results for different single emulsifiers at room temperature (from left to right: 601#, 2301#, by140, 501#, s-20, el-40)
[0038] Figure 2 Experimental results of different single emulsifiers during thermal storage (from left to right: 2301#, by140, 501#, el-40, s-20)
[0039] Figure 3 Graphs of analysis of different single emulsifiers during cold storage (from left to right: 2301#, by140, 501#, el-40, s-20)
[0040] Figure 4 Graphs of emulsifier analysis at room temperature in different ratios of (S-20:EL-40) (from left to right: 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2, 9:1)
[0041] Figure 5 Graphs of emulsifier analysis in different ratios of EL-40:S-20 during cold storage (from left to right: 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2, 9:1)
[0042] Figure 6 Experimental diagrams of emulsifiers with different ratios (EL-40:S-20) during hot storage (from left to right: 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2, 9:1).
[0043] Figure 7 Graph showing foam volume at 0 min for different amounts of defoamer (addition amounts from left to right: 0%, 0.1%, 0.2%, 0.3%)
[0044] Figure 8 Graph showing the foam volume of different amounts of defoamer added at 1 minute (addition amounts from left to right: 0%, 0.1%, 0.2%, 0.3%)
[0045] Figure 9 Graph showing foam volume at 2 minutes for different amounts of defoamer (from left to right: 0%, 0.1%, 0.2%, 0.3%)
[0046] Figure 10 Graph showing foam volume at 3 minutes for different amounts of defoamer (addition amounts from left to right: 0%, 0.1%, 0.2%, 0.3%)
[0047] Figure 11 Graph showing foam volume at 4 minutes for different amounts of defoamer (addition amounts from left to right: 0%, 0.1%, 0.2%, 0.3%)
[0048] Figure 12Graph showing foam volume at 5 minutes for different amounts of defoamer (addition amounts from left to right: 0%, 0.1%, 0.2%, 0.3%)
[0049] Figure 13 Experimental graphs of ethylene glycol with different addition amounts (addition amounts from left to right: 0%, 1%, 2%, 3%, 4%, 5%)
[0050] Figure 14 Particle size determination chart at shear speed of 5000 r / min
[0051] Figure 15 Particle size determination chart at shear speed of 6000 r / min
[0052] Figure 16 Particle size determination chart at shear speed of 7000 r / min
[0053] Figure 17 Particle size determination chart at shear speed of 8000 r / min
[0054] Figure 18 Particle size determination chart at shear speed of 9000 r / min
[0055] Figure 19 Emulsion stability test results (from left to right: no floating oil, no separation, no sedimentation)
[0056] Figure 20 Emulsion dispersibility test graphs (from left to right: before dispersion, during dispersion, after dispersion)
[0057] Figure 21 : Thermal storage stability test diagram (A is the precipitate, B is after shaking)
[0058] Figure 22 Graph showing the low-temperature stability of the emulsion (left: before shaking; right: after shaking)
[0059] Figure 23 Line graph showing the time-dependent effect of capsicum extract emulsion on red mites.
[0060] Figure 24 Comparison of the killing effect of chili pepper extract emulsion on red mites (left image: normally growing red mites, right image: dead red mites turned over). Detailed Implementation
[0061] The technical solution of the present invention will be further described below with reference to specific embodiments, but the scope of protection of the present invention is not limited thereto.
[0062] Example 1: Chili Extract Emulsion
[0063] Formula: 8% wintergreen oil, 2% ethylene glycol, 0.1% defoamer, 10% emulsifier, 2% diluted capsicum extract, and the remainder is water.
[0064] Example 2: Chili Extract Emulsion
[0065] Formula: 6% wintergreen oil, 3% ethylene glycol, 0.2% defoamer, 8% emulsifier, 1% diluted capsicum extract, and the remainder is water.
[0066] Example 3: Chili Extract Emulsion
[0067] Formula: 10% wintergreen oil, 5% ethylene glycol, 0.3% defoamer, 12% emulsifier, 3% diluted capsicum extract, and the remainder is water.
[0068] Example 4: Chili Extract Emulsion
[0069] Formula: 8% wintergreen oil, 3% ethylene glycol, 0.2% defoamer, 10% emulsifier, 2% diluted capsicum extract, and the remainder is water.
[0070] Example 5: Chili Extract Emulsion
[0071] Formula: 8% wintergreen oil, 4% ethylene glycol, 0.3% defoamer, 10% emulsifier, 2% diluted capsicum extract, and the remainder is water.
[0072] Example 6: Chili Extract Emulsion
[0073] Formula: 8% wintergreen oil, 5% ethylene glycol, 0.1% defoamer, 10% emulsifier, 2% diluted capsicum extract, and the remainder is water.
[0074] Example 7: Chili Extract Emulsion
[0075] Formula: 8% wintergreen oil, 2% ethylene glycol, 0.2% defoamer, 10% emulsifier, 2% diluted capsicum extract, and the remainder is water.
[0076] Example 8: Chili Extract Emulsion
[0077] Formula: 8% wintergreen oil, 2% ethylene glycol, 0.3% defoamer, 10% emulsifier, 2% diluted capsicum extract, and the remainder is water.
[0078] Example 9: Chili Extract Emulsion
[0079] Formula: 7% wintergreen oil, 2% ethylene glycol, 0.2% defoamer, 9% emulsifier, 2% diluted chili extract, and the remainder is water.
[0080] Example 10: Chili Extract Emulsion
[0081] Formula: 9% wintergreen oil, 2% ethylene glycol, 0.2% defoamer, 11% emulsifier, 1% capsicum extract dilution, and the remainder is water.
[0082] Example 11: Chili Extract Emulsion
[0083] Formula: 7% wintergreen oil, 3% ethylene glycol, 0.1% defoamer, 9% emulsifier, 3% diluted chili extract, and the remainder is water.
[0084] Example 12: Chili Extract Emulsion
[0085] Formula: 9% wintergreen oil, 3% ethylene glycol, 0.1% defoamer, 11% emulsifier, 2% diluted capsicum extract, and the remainder is water.
[0086] Examples 1-12: Capsicum extract emulsion formulations used in the following preparation methods
[0087] Example 13: Preparation method of chili extract emulsion
[0088] (1) Preparation of dried chili powder: Remove the stems and seeds of dried red chilies, place them in a 50℃ constant temperature drying oven to dry for 2 hours, pulverize them through a 40-mesh sieve, collect the dried chili powder, and set aside for later use.
[0089] (2) Chili extraction: Weigh a certain amount of chili powder, add 95% ethanol at a material-to-liquid ratio of 1:4, extract by ultrasonication for 35 minutes at a power of 90W, filter under normal pressure, add the same volume of 95% ethanol again, ultrasonicate under the same conditions, filter, combine the filtrates, and collect for later use.
[0090] (3) Preparation of chili extract: Collect the filtrate, concentrate it under reduced pressure, manually adjust the water bath temperature to 40℃ and the rotation speed to 60r / min (as ethanol evaporates, the water bath temperature and rotation speed should be gradually increased, manually adjust the temperature and rotation speed, the maximum temperature should not exceed 65℃, and the rotation speed should be controlled at 90r / min). When the filtrate evaporates to 10mL, collect the filtrate, dry the concentrate in a constant temperature oven at 120℃ to constant weight, and obtain the crude chili extract.
[0091] (4) Preparation of chili extract dilution: Take the crude chili extract, add 48.5 mL of wintergreen oil, sonicate to dissolve, and make up to 50 mL to prepare a chili extract dilution with a concentration of 0.03 g / mL for later use. Shake well before each use.
[0092] The volume-to-mass ratio of wintergreen oil to crude chili extract is: wintergreen oil: crude chili extract = 48.5:1.5;
[0093] (5) Preparation of emulsion:
[0094] The diluted chili extract and wintergreen oil were mixed according to the formula ratio. Then, an emulsifier was added as the oil phase and deionized water as the aqueous phase. Ethylene glycol and defoamer were added to the aqueous phase. The aqueous phase was slowly poured into the oil phase while stirring. The mixture was stirred to form a crude emulsion. Then, a high-speed shear emulsifier was used to gradually increase the speed to 9000 r / min for 5 minutes to obtain a stable chili extract emulsion.
[0095] Example 14: Preparation method of chili extract emulsion
[0096] (1) Preparation of dried chili powder: Remove the stems and seeds of dried red chilies, place them in a constant temperature drying oven at 55℃ and dry for 1.5h, pulverize them through a 40-mesh sieve, collect the dried chili powder and set aside.
[0097] (2) Chili extraction: Weigh a certain amount of chili powder, add 95% ethanol at a material-to-liquid ratio of 1:4, extract by ultrasonication for 30 minutes at a power of 80W, filter under normal pressure, add the same volume of 95% ethanol again, ultrasonicate under the same conditions, filter, combine the filtrates, and collect for later use.
[0098] (3) Preparation of chili extract: Collect the filtrate, concentrate it under reduced pressure, manually adjust the water bath temperature to 50℃ and the rotation speed to 70r / min (as ethanol evaporates, the water bath temperature and rotation speed should be gradually increased, manually adjust the temperature and rotation speed, the maximum temperature should not exceed 65℃, and the rotation speed should be controlled at 90r / min), collect the filtrate when the filtrate evaporates to 10mL, dry the concentrate in a constant temperature oven at 120℃ to constant weight, and obtain the crude chili extract;
[0099] (4) Preparation of chili extract dilution: Take the crude chili extract, add 48.5 mL of wintergreen oil, sonicate to dissolve, and make up to 50 mL to prepare a chili extract dilution with a concentration of 0.03 g / mL for later use. Shake well before each use.
[0100] The volume-to-mass ratio of wintergreen oil to crude chili extract is: wintergreen oil: crude chili extract = 48.5:1.5;
[0101] (5) Preparation of emulsion:
[0102] The diluted chili extract and wintergreen oil were mixed according to the formula ratio. Then, an emulsifier was added as the oil phase and deionized water as the aqueous phase. Ethylene glycol and defoamer were added to the aqueous phase. The aqueous phase was slowly poured into the oil phase while stirring. The mixture was stirred to form a coarse emulsion. Then, a high-speed shear emulsifier was used to gradually increase the speed to 8000 r / min for 5 minutes to obtain a stable chili extract emulsion.
[0103] Example 15: Preparation method of chili extract emulsion
[0104] (1) Preparation of dried chili powder: Remove the stems and seeds of dried red chilies, place them in a constant temperature drying oven at 60℃ and dry for 2.5h, pulverize them through a 40-mesh sieve, collect the dried chili powder and set aside.
[0105] (2) Chili extraction: Weigh a certain amount of chili powder, add 95% ethanol at a material-to-liquid ratio of 1:4, extract by ultrasonication for 40 minutes at a power of 100W, filter under normal pressure, add the same volume of 95% ethanol again, ultrasonicate under the same conditions, filter, combine the filtrates, and collect for later use.
[0106] (3) Preparation of chili extract: Collect the filtrate, concentrate it under reduced pressure, manually adjust the water bath temperature to 60℃ and the rotation speed to 80r / min (as ethanol evaporates, the water bath temperature and rotation speed should be gradually increased, manually adjust the temperature and rotation speed, the maximum temperature should not exceed 65℃, and the rotation speed should be controlled at 90r / min). When the filtrate evaporates to 10mL, collect the filtrate, dry the concentrate in a constant temperature oven at 120℃ to constant weight, and obtain the crude chili extract.
[0107] (4) Preparation of chili extract dilution: Take the crude chili extract, add 48.5 mL of wintergreen oil, sonicate to dissolve, and make up to 50 mL to prepare a chili extract dilution with a concentration of 0.03 g / mL for later use. Shake well before each use.
[0108] The volume-to-mass ratio of wintergreen oil to crude chili extract is: wintergreen oil: crude chili extract = 48.5:1.5;
[0109] (5) Preparation of emulsion:
[0110] The diluted chili extract and wintergreen oil were mixed according to the formula ratio. Then, an emulsifier was added as the oil phase and deionized water as the aqueous phase. Ethylene glycol and defoamer were added to the aqueous phase. The aqueous phase was slowly poured into the oil phase while stirring. The mixture was stirred to form a crude emulsion. Then, a high-speed shear emulsifier was used to gradually increase the speed to 9000 r / min for 5 minutes to obtain a stable chili extract emulsion.
[0111] To further verify the feasibility and effectiveness of the present invention and to select the optimal solution, the inventors conducted a series of experiments, as follows:
[0112] Part 1: Preparation of Capsicum Extract Emulsion
[0113] 1. Instruments and Materials
[0114] 1.1 Instruments
[0115] Table 1 Instruments
[0116]
[0117] 1.2 Reagents
[0118] 95% ethanol (batch number: May 25, 2020), wintergreen oil (batch number: by20221214; methyl salicylate), ultrapure water for experiments, concentrated emulsion 601 (tristyrene-based phenol polyoxyethylene ether), by140 (castor oil ethylene oxide adduct), 2301# (polyoxyethylene laurate), EL-40 (nethole oil polyoxyethylene ether), 500# (calcium dodecylbenzene sulfonate), S-20 (sorbitan laurate), defoamer (organosilicon), ethylene glycol (batch number: September 4, 2021), anhydrous calcium chloride (batch number: 2022-12-01), magnesium chloride (batch number: 2022-12-01).
[0119] 1.3 Sample Source
[0120] All medicinal samples in this experiment were dried red chilies purchased by the author from the Qunsheng Dazhihui Yonghui Supermarket in Huaxi District, Guiyang City, and identified by Professor Wei Shenghua of Guizhou University of Traditional Chinese Medicine as the fruit of Capsicum annuum (Linn), a plant belonging to the genus Capsicum in the Solanaceae family.
[0121] 2. Methods and Results
[0122] 2.1 Extraction of dried chili peppers
[0123] 2.1.1 Preparation of dried chili powder
[0124] Remove the stems and seeds from the dried red chilies purchased from the supermarket, place them in a constant temperature drying oven at 50℃ for 2 hours, grind them with a universal grinder, and collect them after passing them through a 40-mesh sieve for later use.
[0125] 2.1.2 Chili Extraction Experiment
[0126] Measure 100 mL of 95% ethanol using a graduated cylinder and add it to a 250 mL Erlenmeyer flask containing 25.00 g of chili powder. Seal the flask with plastic wrap. Place the Erlenmeyer flask in a 90 W ultrasonic cleaner for 35 min. Filter under normal pressure, then add 100 mL of 95% ethanol back to the filter residue along with the filter paper. Repeat the above operation, then combine the two filtrates and collect them for later use.
[0127] 2.1.3 Concentration of Capsicum Extract
[0128] During vacuum concentration, the water bath temperature should initially be controlled at 40℃ and the rotation speed at 60 r / min. As ethanol evaporates, the water bath temperature and rotation speed should be gradually increased, with the maximum temperature not exceeding 65℃ and the rotation speed controlled at 90 r / min. Remove the filtrate when approximately 10 mL has evaporated. Pour the concentrate into a beaker (weigh and record the beaker's weight beforehand), rinse the test tube with anhydrous ethanol to remove any remaining concentrate, combine the filtrate with the excess ethanol evaporated from the water bath, and then dry in a 120℃ constant temperature oven until constant weight. Weigh the total amount and subtract the weight of the beaker to obtain the crude chili extract weight. The chili extract was crudely extracted three times, and the extraction rates are shown in Table 2 below.
[0129] Table 2 Extraction rate of chili extract
[0130]
[0131] 2.1.4 Preparation of dilute solution of capsicum extract
[0132] Take the concentrated and dried chili extract from "2.1.3", add a small amount of wintergreen oil, and place it in an ultrasonic cleaner to accelerate the dissolution of the chili extract. Repeat the operation several times, and bring the volume of the chili extract and wintergreen oil mixture to 50 mL. Shake well before each use. The concentration of chili extract is 0.03 g / mL.
[0133] 2.2 Preparation of Emulsion
[0134] 2.2.1 Screening experiment for emulsifiers
[0135] (1) Screening of emulsifier types
[0136] Referring to Zhang Guisen's development of a 5% rotenone emulsion, a screening experiment was conducted using all available emulsifiers in this experiment. Five emulsifiers were selected: 601 (tristyrylphenol polyoxyethylene ether), BY140 (castor oil ethylene oxide adduct), EL-40 (nethole oil polyoxyethylene ether), 500# (calcium dodecylbenzene sulfonate), S-20 (sorbitan laurate), and 2301# (polyoxyethylene laurate). The emulsifier addition amount was 10% in the emulsion, hence the quantitative measure was 10%. The amount of chili extract solution added was 10%, and ultrapure water was added to bring the volume to 100 mL. The emulsion was prepared using the phase inversion method at 5000 rpm for 5 minutes to obtain a light pink emulsion.
[0137] See Table 3. Figures 1-3 .
[0138] Table 3 Screening of Emulsion Types
[0139]
[0140] According to the literature
[19] According to the judgment criteria, EL-40 and S-20 have good emulsification effects, 601# has no emulsification effect, and 2301#, 5000# and By140 have poor emulsification effects. EL-40 and S-20 can be compounded to reduce the water separation rate.
[0141] (2) Compounding of emulsifiers
[0142] Referring to Zhang Guisen's development of a 5% rotenone emulsion, different emulsifiers have different hydrophilic and lipophilic properties. By compounding emulsifiers, a synergistic effect can be achieved, improving the various properties of the emulsion and the stability of the formulation. The compounding ratios of 8:2 and 4:6 were increased. Based on the two emulsifiers S-20 and E1-40 with low water separation volume obtained from the initial emulsifier screening, compounding ratios of 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2, and 9:1 were selected. A 10% capsicum extract solution was added, and ultrapure water was added to bring the volume to 100 mL. The emulsion was prepared using the phase inversion method at 5000 rpm for 5 minutes to obtain a light pink emulsion.
[0143] See Table 4. Figures 4-6 .
[0144] Table 4 Screening of Emulsifier Compounds
[0145]
[0146] As shown in Table 4, as the proportion of EL-40 increases, the amount of water separation gradually decreases at room temperature, cold storage, and hot storage. Therefore, the emulsifier ratio selected is EL-40:S-20 (9:1).
[0147] 2.2.2 Single-factor experiment to investigate additives in emulsions
[0148] (1) Amount of defoamer added
[0149] During the emulsifier preparation and shearing process, a large number of bubbles are generated and dissipate slowly, increasing the emulsion volume and affecting subsequent experimental observation and judgment. Adding an organosilicon defoamer can quickly dissipate the bubbles, eliminating both large and small bubbles. A single-factor experiment was conducted using the amount of defoamer added as the defoamer, with addition amounts of 0%, 0.05%, 0.1%, 0.2%, and 0.3%. The emulsifier was 10%, the chili extract solution was 10%, and ultrapure water was added to a final volume of 100 mL. The emulsion was prepared using the phase inversion method at 5000 rpm for 5 minutes, yielding a light pink emulsion. See Table 5. Figures 7-12 .
[0150] Table 5. Addition of defoamer
[0151]
[0152] As shown in Table 5, the defoaming rate is not significantly different when the defoamer content is 0.1%, 0.2%, and 0.3%, but the defoaming rate is lower when the defoamer content is 0% and 0.05%. Therefore, the defoamer content of 0.1% is selected.
[0153] (2) Amount of ethylene glycol added
[0154] During cold storage stability testing, the addition of ethylene glycol prevented water and oil separation, while the absence of ethylene glycol resulted in oil and water separation after freeze-thaw cycles. Adding a certain amount of ethylene glycol perfectly resolved these issues. A single-factor experiment was conducted with ethylene glycol addition rates of 0%, 1%, 2%, 3%, 4%, and 5%. The emulsifier was 10%, the chili extract solution was 10%, and ultrapure water was added to a final volume of 100 mL. The emulsion was prepared using a phase inversion method at 5000 rpm for 5 minutes, yielding a light pink emulsion. See Table 6. Figure 13 .
[0155] Table 6 Ethylene glycol addition amount
[0156]
[0157] As shown in Table 6, with the increase of ethylene glycol addition, after freezing at -18℃ and restoring to room temperature, an oil phase will precipitate without the addition of ethylene glycol. With the increase of ethylene glycol addition of 2%, 3%, 4%, and 5%, no oil phase precipitates. Therefore, the addition of 2% ethylene glycol is selected.
[0158] (3) Emulsifier shear speed
[0159] In the preparation of emulsions, the shear speed of the emulsifier affects the stability of the emulsion system. A slow speed results in poor emulsification and prevents the formation of a uniform oil-in-water emulsion. Increasing the shear speed of the emulsifier helps to form a uniformly dispersed emulsion. Single-factor experiments were conducted using shear speeds of 5000 r / min, 6000 r / min, 7000 r / min, 8000 r / min, and 9000 r / min. A light pink emulsion was obtained after shearing for 5 minutes using the phase inversion method. (See Table 7.)
[0160] Table 7. Shear speed of emulsifier
[0161]
[0162] As shown in Table 7, with the increase of rotation speed, the precipitation of oil-free phase in the thermal storage occurs after 8000 r / min.
[0163] (4) Particle size determination
[0164] The size and span of the particle size in the emulsion can indicate the stability of the emulsion. The smaller the span, the more stable the system. The particle size of the prepared pepper extract emulsion was measured using a zeta potential and nanoparticle size analyzer. The particle size distribution of the emulsion is represented by δ. D10, D50, and D90 are the average particle sizes of the preparation corresponding to 10%, 50%, and 90% of the cumulative distribution curve of the emulsion. The smaller the δ value [(D90 - D10) / D50], the better. A small δ value indicates a narrow particle size distribution, good dispersion performance, and good stability of the prepared emulsion.
[0165] See Table 7 and Table 8; see Figures 14-18 .
[0166] Table 8 Particle Size Determination
[0167]
[0168] As can be seen from Table 7 and Table 8, as the rotation speed increases, no oil phase separation occurs in the heat storage at 8000 r / min and 9000 r / min, and the particle size span is small at 9000 r / min, and the emulsion system is more stable.
[0169] 2.2.3 Stability Determination Experiment in Emulsion
[0170] (1) Determination of Emulsion Stability
[0171] Preparation of standard hard water: Weigh 0.304 g of anhydrous calcium chloride and 0.139 g of magnesium chloride with crystal water in a 1000 mL volumetric flask, dissolve with distilled water and dilute to the mark for standby.
[0172] In accordance with GB / T 1603—2001 "Determination Method for Emulsion Stability of Pesticides", the emulsion sample was diluted 200 times in standard hard water, observed after standing for 1 h. If there is no floating oil on the upper layer, no precipitation on the lower layer, and no stratification, the emulsion stability is qualified. See Figure 19 .
[0173] (2) Determination of Emulsion Dispersibility
[0174] The emulsion sample was added to the standard hard water, and its ability to form an emulsion in hard water was observed. If it immediately shows a cloudy state when dropped into water, it is judged as excellent; if there are particles sinking but can be basically dispersed, it is judged as good; if it needs to be shaken to disperse, it is judged as medium; if it sinks in a flocculent state and cannot be automatically dispersed and needs to be strongly shaken, it is judged as poor. See Figure 20 .
[0175] (3) Determination of Emulsion Thermal Storage Stability
[0176] It is carried out according to the method in GB / T 19136—2003 "Determination Method for Thermal Storage Stability of Pesticides". Add the emulsion sample into a test tube and seal it. Each sample is repeated 3 times. Put it into an incubator at (54±2)°C. After 14 days, observe that there is no precipitation or oil separation. If there is a small amount, gently shake it to mix evenly, and it is judged as qualified. Calculate the oil separation volume. If it is oil droplets, suck it out with a graduated dropper. If it is at the lower layer, measure the volume length of the separated oil with a graduated test tube and divide it by the total length. The precipitation rate is the precipitation volume / total volume, and the precipitation rate can be obtained. See Table 9. See Figure 21 .
[0177] Table 9 Determination of Thermal Storage Stability
[0178]
[0179] As can be seen from Table 9, a small amount of precipitates disappear after shaking, and the thermal storage stability is qualified.
[0180] (4) Determination of Low Temperature Stability of Emulsion
[0181] It is carried out according to Method 2.1 in GB / T 19137—2003 "Determination Method for Low Temperature Stability of Pesticides". Seal the emulsion sample. Each sample is repeated 3 times. Place it in a refrigerator at (0±2)°C for 7 days. Observe that there is no oil separation and the precipitates do not exceed 0.3 mL, which is qualified. Since there is no 100 mL centrifuge tube, use a 1.5 mL centrifuge tube. Calculate the precipitate volume by weight, that is, the precipitation rate does not exceed 0.3%. Add 1 mL of emulsion for a 7-day low temperature stability test. Weigh the centrifuge tube, the weight of the added emulsion, and the centrifuge tube containing the precipitate after centrifugation. (Centrifuge tube containing the precipitate after centrifugation - centrifuge tube weight) / weight of the emulsion to obtain the centrifugation rate. See Table 10. See Figure 22 .
[0182] Table 10 Determination of Low Temperature Stability of Emulsion
[0183]
[0184] As can be seen from Table 10, the precipitation rates do not exceed 0.3%, and the cold storage stability is qualified.
[0185] 2.2.4 Preparation Method of Emulsion
[0186] The formula of the pepper extract emulsion is: active ingredient of the technical material (diluted solution of pepper extract) 2%, organic solvent (wintergreen oil) 8%, surfactant (EL-40:S-20 (9:1) 10%, antifreeze (ethylene glycol) 2%, other auxiliaries and additives (ethylene glycol) 0.3%, defoamer 0.1%, water (ultrapure water) is made up to 100 mL.
[0187] The emulsion was prepared by phase inversion method. 2 mL of diluted chili extract was mixed with 8 mL of wintergreen oil, and then an emulsifier was added as the oil phase and deionized water as the aqueous phase. 2 mL of ethylene glycol and 0.1 g of defoamer were added to the aqueous phase. The aqueous phase was slowly poured into the oil phase while stirring. The mixture was stirred to form a crude emulsion. The emulsion was then sheared and emulsified for 5 min using a high-speed shear emulsifier, with the speed gradually increased to 9000 r / min, to obtain a stable chili extract emulsion.
[0188] 3. Conclusion
[0189] Five emulsifiers—601#, by140, el-40, 5011, 500#, and S-20—were screened in section “2.2.1”. Table 1 shows that by140, el-40, 2301, 500#, and S-20 all exhibited emulsifying properties. However, By140, 2301, and 500# failed the hot and cold storage stability tests, and 601 did not perform any emulsifying function, so no hot or cold storage tests were conducted. A compounding experiment was conducted using S-20 and el-40. Table 2 shows that the emulsion tended to stabilize as the amount of el-40 increased. A 9:1 (el-40:S-20) emulsifier ratio was selected.
[0190] Freeze-thaw experiments were conducted without adding ethylene glycol as described in section "2.2.2". Adding ethylene glycol reduced oil precipitation; therefore, 2% ethylene glycol was selected to determine the appropriate dosage. Without defoamer, numerous bubbles were generated during the emulsifier preparation shearing process, dissipating slowly and increasing emulsion volume, affecting subsequent experimental observation and judgment. Adding an organosilicon defoamer resulted in rapid bubble dissipation and the elimination of bubbles of varying sizes. Therefore, 0.1% defoamer was selected to determine the appropriate dosage. Thermal stability tests revealed that increasing rotational speed improved emulsification between the emulsifier and the oil phase, resulting in uniform dispersion in the aqueous phase. Oil precipitation occurred to varying degrees at speeds between 5000-7000 rpm, but no oil precipitation occurred after 8000 rpm. At 9000 rpm, the particle size distribution was small, and the emulsion was more stable.
[0191] In section "2.2.3", the performance indicators of the emulsion were examined. The emulsion sample was diluted 200 times in standard hard water and observed after standing for 1 hour. No floating oil, no sediment, and no stratification were observed, indicating that the emulsion stability was qualified. However, the emulsion dispersibility was good; some particles settled but were basically dispersed, which was considered good. For thermal storage stability testing, a small amount of oil separation was observed, but after gentle shaking and thorough mixing, the emulsion's thermal storage stability was qualified. For low-temperature stability testing, after being placed in a refrigerator at (0±2)℃ for 7 days, no oil separation was observed, and the centrifugal precipitate did not exceed 0.3%, indicating that the emulsion's low-temperature stability was qualified.
[0192] The chili extract emulsion formulation is as follows: 8% wintergreen oil, 2% ethylene glycol, 0.1% defoamer, 10% (EL-40:S-20 = 9:1) emulsifier, 2 mL chili extract diluent, and ultrapure water to a final volume of 100 mL. This emulsion formulation has passed stability tests, including heat storage stability and cold storage stability tests, and is therefore a qualified emulsion. See Table 11.
[0193] Table 11 Detection results of chili extract emulsion indicators
[0194]
[0195]
[0196] Part Two: Evaluation of the Insecticidal Efficacy of Chili Extract Emulsion
[0197] 1. Instruments and Materials
[0198] 1.1 Instruments
[0199] Electronic analytical balance (Mettler-Toledo, Switzerland), electrically heated constant temperature drying oven (manufactured by Changsha Instrument Factory); ultrapure water for experiments, electron microscope.
[0200] 2. Methods and Results
[0201] 2.1 Effects and Statistical Analysis of Chili Extract Emulsion on Pests
[0202] 2.2.1 Screening of working concentrations of chili extract
[0203] Following the emulsion formulations selected in Part 1, the total oil phase was 10%. The oil phase (wintergreen oil + diluted chili extract) was further prepared by adding 2 mL, 4 mL, 6 mL, and 8 mL of diluted chili extract, respectively, using a phase inversion method to create 100 mL chili extract emulsions. Ten azalea plants were taken from each group and labeled accordingly. Based on concentration, the groups were labeled L1, L2, L3, and L4, for a total of four groups. Each group was diluted 1000 times, with a spacing of more than 2 meters between groups. The pesticide was sprayed evenly on both sides of the leaves. See Table 12.
[0204] Table 12 Screening of working concentrations of chili extract
[0205]
[0206] 2.1.2 Pest mortality and repulsion
[0207] Before spraying the chili extract emulsion, the number of red mites on each azalea plant was observed and recorded. Three azalea plants were randomly selected from each group using a random sampling method to count the number of red mites on the leaves. The average number of red mites on each group of azalea plants was obtained: 66 in L1, 69 in L2, 74 in L3, and 59 in L4.
[0208] One day after spraying the chili extract emulsion, three plants were randomly selected from each group for observation and statistical analysis. The average number of red mites on each group of azaleas was obtained. The average number of surviving red mites on azaleas in L1 was 56, with a repellency and killing rate of 15.2%; the average number of red mites on azaleas in L2 was 58, with a repellency and killing rate of 15.9%; the average number of red mites on azaleas in L3 was 62, with a repellency and killing rate of 16.2%; and the average number of red mites on azaleas in L4 was 46, with a repellency and killing rate of 22.0%.
[0209] Two days after spraying the chili extract emulsion, three plants were randomly selected from each group for observation and statistical analysis. The average number of red mites on each group of azaleas was obtained. In L1, the average number of surviving red mites on azaleas was 44, with a repellency and killing rate of 33.3%; in L2, the average number of red mites on azaleas was 45, with a repellency and killing rate of 34.8%; in L3, the average number of red mites on azaleas was 48, with a repellency and killing rate of 35.1%; and in L4, the average number of red mites on azaleas was 31, with a repellency and killing rate of 47.5%.
[0210] Three days after spraying the chili extract emulsion, three plants were randomly selected from each group for observation and statistical analysis. The average number of red mites on each group of azaleas was obtained. In L1, the average number of surviving red mites on azaleas was 31, with a repellency and killing rate of 53.0%; in L2, the average number of red mites on azaleas was 31, with a repellency and killing rate of 55.0%; in L3, the average number of red mites on azaleas was 33, with a repellency and killing rate of 55.4%; and in L4, the average number of red mites on azaleas was 15, with a repellency and killing rate of 74.6%.
[0211] Four days after spraying with chili extract emulsion, three plants were randomly selected from each group for observation and statistical analysis. The average number of red mites on each group of azaleas was obtained. In L1, the average number of surviving red mites on azaleas was 16, with a repellency and killing rate of 75.8%; in L2, the average number of red mites was 15, with a repellency and killing rate of 78.3%; in L3, the average number of red mites was 16, with a repellency and killing rate of 78.4%; and in L4, the average number of red mites was 3, with a repellency and killing rate of 94.9%.
[0212] Five days after spraying with chili extract emulsion, three plants were randomly selected from each group for observation and statistical analysis. The average number of red mites on each group of azaleas was obtained. Because the eggs of red mites hatch into new red mites, the number of red mites increased. The average number of surviving red mites on the azaleas in L1 was 34, with a repellency and killing rate of 50.7%; the average number of red mites on the azaleas in L2 was 32, with a repellency and killing rate of 53.6%; the average number of red mites on the azaleas in L3 was 33, with a repellency and killing rate of 55.4%; and the average number of red mites on the azaleas in L4 was 21, with a repellency and killing rate of 64.4%.
[0213] Six days after spraying with chili extract emulsion, three plants were randomly selected from each group for observation and statistical analysis. The average number of red mites on each group of azaleas was obtained. In L1, the average number of surviving red mites on azaleas was 22, with a repellency and killing rate of 66.7%; in L2, the average number of red mites was 19, with a repellency and killing rate of 72.5%; in L3, the average number of red mites was 19, with a repellency and killing rate of 74.3%; and in L4, the average number of red mites was 6, with a repellency and killing rate of 89.8%.
[0214] Seven days after spraying with chili extract emulsion, three plants were randomly selected from each group for observation and statistical analysis. The average number of red mites on each group of azaleas was obtained. Because the eggs of red mites hatch into new red mites, the number of red mites increased. The average number of surviving red mites on the azaleas in L1 was 9, with a repellency and killing rate of 86.4%; the average number of red mites on the azaleas in L2 was 5, with a repellency and killing rate of 92.8%; the average number of red mites on the azaleas in L3 was 4, with a repellency and killing rate of 94.6%; and the average number of red mites on the azaleas in L4 was 3, with a repellency and killing rate of 95.0%.
[0215] Eight days after spraying with chili extract emulsion, three plants were randomly selected from each group for observation and statistical analysis. The average number of red mites on each group of azaleas was obtained. Because the eggs of red mites hatch into new red mites, the number of red mites increased. The average number of surviving red mites on the azaleas in L1 was 4, with a repellency and killing rate of 94.0%; the average number of red mites on the azaleas in L2 was 4, with a repellency and killing rate of 94.2%; the average number of red mites on the azaleas in L3 was 5, with a repellency and killing rate of 93.2%; and the average number of red mites on the azaleas in L4 was 4, with a repellency and killing rate of 93.2%.
[0216] 2.1.3 Statistical analysis of the duration of action of chili extract emulsion
[0217] Based on long-term observation after spraying the chili extract emulsion, the recurrence of red mites was infrequent, with only a small number of active red mites present. No large-scale outbreaks occurred, and no traces of red mites were found after 15 days. This may be because the weather affected the activity of the red mites, preventing their detection.
[0218] 3. Conclusion
[0219] The number of red mites decreased continuously from day 1. New red mites hatched on day 5, and were repelled and killed after 2 days. After 8 days, the repellency and killing rate of red mites reached over 90%, achieving the effects of rendering the mites inactive, non-feeding, dead, and repelled. Furthermore, even with new red mites hatching, they could still be repelled and killed by the chili pepper extract emulsion, indicating that the chili pepper extract emulsion has a long-lasting effect and is effective in the outbreak and prevention of red mite outbreaks. The trend of its effect is as follows. Figure 23 As shown in the figure, the effect of chili extract on red mites is illustrated in the image. Figure 24 As shown.
[0220] Although the present invention has been described in detail above with general descriptions, specific embodiments, and experiments, modifications or improvements can be made to it, which will be obvious to those skilled in the art. Therefore, all such modifications or improvements made without departing from the spirit of the present invention fall within the scope of protection claimed by the present invention.
Claims
1. A method for preparing a pepper extract emulsion having a red mite of Chinese herbal medicine preventing or killing effect, characterized in that, It comprises the following steps: Mix 1-3% pepper extract diluent with 6-10% wintergreen oil, then add 8-12% emulsifier as oil phase, select deionized water as water phase, add 2-5% ethylene glycol in the water phase, 0.1-0.3% silicone antifoaming agent, slowly pour the water phase into the oil phase while stirring, stir to form a coarse emulsion, then use a high-speed shearing emulsifier, gradually increase the speed to 8000-9000r / min, shear emulsify for 5 min, and then a stable pepper extract emulsion is obtained; the emulsifier is EL-40:S-20=9:1; The preparation method of the pepper extract diluent comprises the following steps: (1) Preparation of dry chili powder: remove the stems and seeds of dry red chilies, place them in a constant temperature drying oven at 50-60°C for 1.5-2.5h, crush them through a 40-mesh sieve, collect the dry chili powder, and reserve it for use; (2) Pepper extraction: weigh a certain amount of chili powder, add 95% ethanol solution according to the solid-liquid ratio of 1:4, ultrasonic extraction, normal pressure filtration, add the same volume of ethanol solution again, ultrasonic extraction under the same conditions, filtration, and collect the filtrate for use; (3) Preparation of pepper extract: collect the filtrate, reduce the pressure for concentration, manually adjust the water bath temperature to control it at 40-65°C, control the rotation speed at 60-90r / min, collect the filtrate when the filtrate is volatilized to 10mL, dry it in a constant temperature oven at 120°C until the weight is constant, and obtain the crude pepper extract; (4) Preparation of pepper extract diluent: take the crude pepper extract, add 48.5mL wintergreen oil, ultrasonic dissolution, and constant volume to 50mL to prepare a pepper extract diluent with a concentration of 0.03g / mL, and reserve it for use, shake it well before each use.
2. The method of claim 1, wherein the preparation method of the capsicum extract emulsion having a red mite prevention or killing effect of Chinese medicinal materials is characterized by, When using the high-speed shearing emulsifier, gradually increase the speed to 9000r / min for shearing emulsification for 5 min.
3. The method of claim 1, wherein the preparation method of the emulsion of the Capsicum annuum L. extract having a preventive or killing effect on the red spider mites of Chinese herbal medicines is characterized by, It comprises the following raw materials in mass percentage: 7-9% wintergreen oil, 2-3% ethylene glycol, 0.1-0.2% antifoaming agent, 9-11% emulsifier, 1-2% pepper extract diluent, and the balance is deionized water.
4. The method of claim 1 or 2, wherein the preparation method of the emulsion of the Capsicum extract having a red mite-preventing or -killing effect of Chinese medicinal materials, is characterized by, It comprises the following raw materials in mass percentage: 8% wintergreen oil, 2% ethylene glycol, 0.1% antifoaming agent, 10% emulsifier, 2% pepper extract diluent, and the balance is deionized water.
5. The application of the pepper extract emulsion prepared by the preparation method of the pepper extract emulsion with red mite prevention or killing effect of traditional Chinese medicinal materials according to any one of claims 1-4 in the preparation of biological pesticide insecticides for preventing or killing red mite pests of traditional Chinese medicinal materials.
Citation Information
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