Cinnamomum camphora extract as well as preparation method and application thereof in mosquitocide
By extracting lignans from camphor tree branches after the natural borneol has been extracted, camphor tree extract was prepared for use as a mosquito repellent, which solved the problems of resource waste and environmental pollution and provided an efficient mosquito control solution.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-29
- Publication Date
- 2026-03-31
AI Technical Summary
In existing technologies, the use of camphor tree branches and leaves after extracting natural borneol is a serious waste of resources, and traditional insecticides pose environmental pollution and health risks, and the problem of preventing and controlling mosquito-borne diseases has not been effectively solved.
Lignans were extracted from camphor tree branches after natural borneol extraction using ultrasonic extraction to prepare camphor tree extract, which was then applied to mosquito repellents. The extraction process was optimized to improve the extraction rate of lignans and the mosquito-killing effect.
This approach enables the high-value utilization of camphor branches, provides an environmentally friendly mosquito repellent, solves the problem of resource waste, and enhances the environmental protection effect of mosquito control.
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Figure CN121753835A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of plant extraction technology, and particularly relates to a camphor camphor extract, its preparation method, and its application in mosquito repellents. Background Technology
[0002] Natural borneol is a precious resource with both medicinal and aromatic value, widely used in the pharmaceutical and high-end daily chemical industries. Its main extraction source is the branches and leaves of camphor tree (Cinnamomum camphora), driving the development of the camphor tree planting and processing industry chain. However, the current processing of camphor tree presents a problem of resource waste: most of the camphor tree branches and leaves after extracting natural borneol are discarded or burned, without being recycled or utilized. This not only violates the concept of green development but also causes secondary environmental pollution.
[0003] Mosquitoes are vectors for many diseases, including dengue fever and malaria, posing a serious threat to public health. Currently, mainstream synthetic insecticides suffer from problems such as cumulative environmental pollution, harmful residues, and the development of insecticide resistance in mosquitoes. Natural plant-derived insecticides offer advantages such as good environmental compatibility, low toxicity, and low resistance to insecticides. Therefore, there is an urgent need to develop natural plant-derived insecticides. The branches and leaves of camphor trees, after the extraction of natural borneol, are rich in lignans and possess mosquito-killing activity. Summary of the Invention
[0004] To address the shortcomings of existing technologies, this invention provides a camphor tree extract, its preparation method, and its application in mosquito repellents, aiming to solve the problems mentioned in the background art.
[0005] In a first aspect, the present invention provides a method for preparing camphor camphor extract, comprising the following steps: drying and pulverizing camphor camphor branches after natural borneol extraction to obtain camphor camphor branch powder; adding camphor camphor branch powder to an extraction solvent, performing ultrasonic extraction, and filtering to obtain camphor camphor extract containing lignans.
[0006] Furthermore, the ratio of camphor twig powder to extraction solvent is 1g: 14-14.5mL.
[0007] Furthermore, the extraction solvent is methanol.
[0008] Furthermore, the temperature for ultrasonic extraction is 45-55℃.
[0009] Furthermore, the ultrasonic extraction time is 55-65 minutes.
[0010] Furthermore, the camphor branches were dried in an oven at 50°C for 24 hours.
[0011] Secondly, the present invention provides a camphor camphor extract, which is prepared by a method for preparing camphor camphor extract.
[0012] Furthermore, the total content of sesamin and 9-hydroxysesamin was used as the evaluation index for the lignan extraction rate of camphor camphor extract.
[0013] Furthermore, the application of camphor camphor extract in mosquito repellents.
[0014] Furthermore, the concentration of camphor camphor extract is 10-100 mg / L.
[0015] The present invention has the following beneficial effects: (1) To improve the residual value of camphor tree branches after the extraction of natural borneol, the rich lignan components are extracted in a targeted manner to solve the problem of resource waste in the traditional natural borneol processing, so as to enable the camphor tree resource to be developed and utilized in a whole-chain, high-value-added manner. The lignans in camphor tree extract, as natural plant-derived mosquito-killing components, have the advantages of good environmental compatibility, no chemical residue risk and compliance with the concept of green prevention and control, providing a sustainable and environmentally friendly solution for mosquito control.
[0016] (2) The extraction process was optimized through single-factor experiments. Methanol was determined to be the best extraction solvent, 50℃ was the optimal extraction temperature, 60min was the optimal extraction time, and 1g:14-14.5mL was the ideal material-liquid ratio. In addition, the total content of sesamin and 9-hydroxysesamin was used as the evaluation index of the lignan extraction rate in camphor camphor extract, which can accurately quantify the lignan content. Attached Figure Description
[0017] Exemplary embodiments of the present invention can be more fully understood by referring to the following figures: Figure 1 This is the mixed control standard of the present invention. and HPLC chromatograms at different injection volumes; Figure 1 A in the text is ; Figure 1 B in the text is .
[0018] Figure 2 This is the standard curve of sesamin, the reference standard of this invention.
[0019] Figure 3 This is the standard curve of 9-hydroxysesamoid, the reference standard of the present invention.
[0020] Figure 4 The results show the lignan extraction rates of each extraction solvent in Example 1 of this invention.
[0021] Figure 5 These are the lignan extraction rates at various extraction times in Example 2 of this invention.
[0022] Figure 6These are the lignan extraction rates at various extraction temperatures in Example 3 of this invention.
[0023] Figure 7 This is the result of lignan extraction rate for each material-liquid ratio in Example 4 of the present invention.
[0024] Figure 8 These are the mosquito-killing activity results of camphor twig extracts from various extraction solvents in Example 6 of the present invention. Detailed Implementation
[0025] To make the technical problems to be solved, the technical solutions, and the beneficial effects of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present invention and are not intended to limit the present invention.
[0026] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains; the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the invention.
[0027] This invention provides a method for preparing camphor camphor extract, comprising the following steps: drying and pulverizing camphor camphor branches after extraction of natural borneol to obtain camphor camphor branch powder; adding camphor camphor branch powder to an extraction solvent, performing ultrasonic extraction, and filtering to obtain camphor camphor extract containing lignans.
[0028] In some embodiments, the ratio of camphor twig powder to extraction solvent is 1g: 14-14.5mL.
[0029] In some embodiments, the extraction solvent is methanol.
[0030] In some embodiments, the temperature for ultrasonic extraction is 45-55°C.
[0031] In some embodiments, the ultrasonic extraction time is 55-65 min.
[0032] In some embodiments, camphor branches are dried in an oven at 50°C for 24 hours.
[0033] In some embodiments, the present invention provides a camphor camphor extract, which is prepared by a method for preparing camphor camphor extract.
[0034] In some embodiments, the total content of sesamin and 9-hydroxysesamin is used as an evaluation index for the lignan extraction rate in camphor camphor extract.
[0035] In some embodiments, the use of a camphor camphor extract in a mosquito repellent.
[0036] In some embodiments, the concentration of camphor camphor extract is 10-100 mg / L.
[0037] In some embodiments, the method for determining the content of lignans (total lignans) is as follows: The total content of sesamin and 9-hydroxysesamin was used as the evaluation index for the lignan extraction rate of camphor camphor extract.
[0038] Preparation of reference solutions and construction of standard curves: Weigh 25.0 mg of sesamin and 12.0 mg of 9-hydroxysesamin, respectively, add acetonitrile and dilute to 5 mL to prepare their respective reference stock solutions. Mix 1.0 mL of each reference stock solution to obtain a sesamin content of 2.5 mg / mL. -1 The content of 9-hydroxysesamin is 1.20 mg·mL. -1 A mixed reference solution (H1) was prepared; 0.4 mL of each reference stock solution was accurately measured, mixed, and diluted to 5 mL to obtain a sesamin content of 0.40 mg / mL. -1 The content of 9-hydroxysesamin was 0.19 mg·mL. -1 A mixed reference solution (H2) was prepared. Mixed reference solutions H1 and H2 were analyzed under HPLC conditions, with 2, 4, 6, 8, and 10 µL of each solution injected to determine peak areas. Standard curves were plotted with peak area on the ordinate and the two concentrations of the reference standard on the abscissa. The HPLC analysis conditions were as follows: a YMC C18 analytical reversed-phase column (150 mm × 4.6 mm, 5 µm) was used, with acetonitrile (A) – water (B) as the mobile phase, gradient elution (0–15 min, 35% A → 55% A; 15–25 min, 55% A → 75% A), and a flow rate of 1.0 mL / min. -1 The detection wavelength was set to 235 nm, the column temperature to 30 °C, and the injection volume to 5 µL.
[0039] The HPLC chromatograms of the mixed reference standards H1 and H2 at different injection volumes are shown below. Figure 1 As shown, Figure 1 The results showed that at a wavelength of 235 nm, 1 was 9-hydroxysematin and 2 was sesamin. The results showed that 9-hydroxysematin and sesamin could be well separated at a detection wavelength of 235 nm, with a separation degree higher than that of 2, and retention times of 11.5 min and 18.0 min, respectively.
[0040] The standard curve of the reference standard sesamin is as follows: Figure 2 As shown, the standard curve of the reference standard 9-hydroxysesamine is as follows: Figure 3As shown. The linear regression equation of the standard curve for sesamin is: y = 1.9848x + 0.8426, R² = 0.99974; the linear regression equation of the standard curve for 9-hydroxysesamin is: y = 0.3857x + 0.26995, R² = 0.99996.
[0041] Example 1: Borneol camphor branches (provided by Jiangxi Jinggangyuan Natural Medicine Co., Ltd.) after natural borneol extraction were dried in an oven at 50℃ for 24 hours. The dried branches were then pulverized using a high-speed universal pulverizer. 1.00g of the borneol camphor branch powder was weighed and placed in a 50mL centrifuge tube. The ratio of borneol camphor branch powder to extraction solvent was 1:10 (g·mL⁻¹). -1 Extraction was carried out at a temperature of 50℃ and an extraction time of 60 min. The extraction solvents were anhydrous ethanol, methanol, acetone, dichloromethane, and ethyl acetate, respectively. The extraction was performed by ultrasonic extraction and filtration to obtain camphor extract (extract) containing lignans.
[0042] The lignan extraction rates for each extraction solvent are as follows: Figure 4 As shown in the figure, the results indicate that when methanol is used as the extraction solvent, the extraction rate of lignans is significantly higher than that of acetone and ethyl acetate (P < 0.01), and significantly higher than that of anhydrous ethanol and dichloromethane (P < 0.05).
[0043] Example 2: After extracting natural borneol, the camphor tree branches were dried in a 50℃ oven for 24 hours. The dried branches were then pulverized using a high-speed universal pulverizer. 1.00 g of camphor tree branch powder was weighed and placed in a 50 mL centrifuge tube. The ratio of camphor tree branch powder to extraction solvent was 1:10 (g·mL⁻¹). -1 The extraction was carried out at a temperature of 50℃ with methanol as the extraction solvent. The extraction time was set to 30, 45, 60, 75 and 90 min respectively. Ultrasonic extraction was performed, followed by filtration to obtain camphor extract containing lignans.
[0044] The lignan extraction rates at different extraction times are as follows: Figure 5 As shown in the figure, the results showed that the lignan extraction rate first increased and then decreased with the extension of extraction time; when the extraction time was 60 min, the lignan extraction rate was the highest, which was significantly higher than that of 30 min (P<0.01), and significantly higher than that of 45 min and 90 min (P<0.05).
[0045] Example 3: After extracting natural borneol, the camphor tree branches were dried in a 50℃ oven for 24 hours. The dried branches were then pulverized using a high-speed universal pulverizer. 1.00 g of camphor tree branch powder was weighed and placed in a 50 mL centrifuge tube. The ratio of camphor tree branch powder to extraction solvent was 1:10 (g·mL⁻¹). -1Extraction was performed at 35, 50, 65, 80 and 95 °C using methanol as the extraction solvent and an extraction time of 60 min. The extraction was followed by ultrasonic extraction and filtration to obtain camphor extract containing lignans.
[0046] The results of lignan extraction rates at various extraction temperatures are as follows: Figure 6 As shown in the figure, the results indicate that the lignan extraction rate first increases and then decreases with increasing extraction temperature; the lignan extraction rate is highest at an extraction temperature of 50℃, which is significantly higher than that at 35℃, 65℃, 80℃ and 95℃ (P<0.01).
[0047] Example 4: After extracting natural borneol, camphor branches were dried in an oven at 50℃ for 24 hours. The dried branches were then pulverized using a high-speed universal pulverizer. 1.00 g of camphor branch powder was weighed and placed in a 50 mL centrifuge tube. Under the conditions of an extraction time of 60 min and methanol as the extraction solvent, the material-to-liquid ratio (camphor branch powder: extraction solvent) was set to 1:6, 1:10, 1:14, 1:18, and 1:22 (g·mL⁻¹). -1 The lignans were extracted by ultrasonic extraction and filtered to obtain camphor camphor extract containing lignans.
[0048] The results of lignan extraction rates for different material-to-liquid ratios are as follows: Figure 7 As shown, the results indicate that the extraction rate of lignans first increases and then decreases with decreasing material-to-liquid ratio, reaching a minimum at 1:14 (g·mL⁻¹). -1 The maximum value is achieved when the material-to-liquid ratio is 1:14 (g·mL). -1 At the same ratio, the extraction rate of lignans was significantly higher than that at 1:6, 1:10, 1:18, and 1:22 (g·mL⁻¹). -1 ).
[0049] Example 5: After extracting natural borneol, camphor tree branches were dried in an oven at 50℃ for 24 hours. The dried branches were then pulverized using a high-speed universal pulverizer. 1.00 g of camphor tree branch powder was weighed and placed in a 50 mL centrifuge tube. The extraction solvent was methanol, and the solid-liquid ratio was 1:14.2 (g·mL⁻¹). -1 The extract was subjected to ultrasonic extraction at 50℃ for 63 minutes, filtered, and the camphor camphor extract containing lignans was obtained.
[0050] The lignan extraction rate was 0.7091%.
[0051] Example 6: Mosquito-killing experiment of total lignan extract: (1) Bioassays were performed using 24-well plates, each containing 2 mL of distilled water. The camphor twig extracts of each extraction solvent were added to dimethyl sulfoxide (DMSO) and piped into the wells to prepare the final target concentrations (1000, 100, 50, 25 and 10 mg / L). A negative control (1% DMSO, without any extract) was set up. (2) 25 fourth-instar larvae were transferred to the holes and the mortality rate was recorded after 24 hours. If there was no reaction when the larvae were touched with a soft plastic dropper, they were considered dead. During the bioassay, no food was provided to the larvae. Three bioassays were conducted independently to determine the toxicity of different solvent camphor twig extracts to mosquito larvae.
[0052] The mosquito-killing activity results of camphor twig extracts extracted with different solvents are as follows: Figure 8 As shown, the results indicate that the mosquito-killing rate of camphor tree branch extracts in various extraction solvents was 1000 mg / L. The mosquito-killing rate decreased to varying degrees with decreasing concentration of camphor tree branch extracts, exhibiting a concentration-dependent effect. The mosquito-killing rate of camphor tree branch extracts in anhydrous ethanol, dichloromethane, and ethyl acetate decreased rapidly at a concentration of 50 mg / L. 50 The LC50 of borneol camphor branch extract in acetone is 50-100 mg / L. 50 Compared to methanol-based camphor twig extracts (25-50 mg / L), this one exhibited the strongest mosquito-killing activity (LC50). 50 The concentration is 10 mg / L.
[0053] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A method of preparing camphor camphor extract, characterized by: The method comprises the following steps: The dried Cinnamomum camphora branches after extraction of natural borneol are crushed to obtain Cinnamomum camphora branch powder; the Cinnamomum camphora branch powder is added into an extraction solvent to perform ultrasonic extraction, and then filtered to obtain a Cinnamomum camphora extract containing lignans.
2. The production method according to claim 1, characterized by: Cinnamomum camphora branch powder: extraction solvent = 1 g: 14-14.5 mL.
3. The production method according to claim 2, characterized by: The extraction solvent is methanol.
4. The production method according to claim 3, characterized by: The temperature of ultrasonic extraction is 45-55 ℃.
5. The production method according to claim 4, characterized by: The time of ultrasonic extraction is 55-65 min.
6. The production method according to claim 5, characterized by: The Cinnamomum camphora branches are dried in an oven at 50 ℃ for 24 h.
7. An extract of Cinnamomum loureiroi, characterized in that: Prepared by the preparation method in any one of claims 1-6.
8. The extract of Cinnamomum camphora according to claim 7, characterized by: The total content of sesamin and 9-hydroxysesamin is used as an evaluation index of the lignan extraction rate in the Cinnamomum camphora extract.
9. The Cinnamomum camphora extract in claim 7 or 8 is used in a mosquito killer.
10. Use according to claim 9, wherein: The concentration of the Cinnamomum camphora extract is 10-100 mg / L.