• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present invention consists of a formulation of a product for application within the agricultural sector mainly, based on a citron limonene extract combined with acetic acid as an emulsifier for use as a natural insecticide on crop pests. The results show that it is an effective combination achieving rates of up to 100% for aphids and whiteflies after one week of application. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2749225A2
    申请号:ES201700146
    申请日:2017-02-18
    公开日:2020-03-19
    发明作者:Bruna Nuria Marti；Lopez Domingo Saura；Segura Carlos Mirabet；Gongora José Manuel Dona；Roldan Jesús Tómas Olivares；Roche Manuel Valero；Botella Sara Gea；Munoz David Mula；Molina Vicente Micol；Castillo Belda Roig Mari Del；Mendoza Elena Cortes
    申请人:Mitra Sol Technologies SL；
    IPC主号:
    专利说明:

    [0001] Synergistic combination of vinegar insecticide and citrus essential oil Technique sector
    [0002] The present invention consists of a formulation of a product for application within the agricultural sector, based on a compound of the essential oils of citrus, limonene, combined with a derivative of vinegar for use as a natural insecticide on crop pests.
    [0003]
    [0004] State of the art
    [0005] The citrus peel has a large number of compounds that can be obtained and used for commercial purposes. The oil contained in bags located on the outside of the fruit mesocarp can be released by breaking them. According to several authors, citrus essential oil is a mixture of volatile compounds and consists mainly of monoterpene hydrocarbons, which have a high level of unsaturation ( Stashenko et al., 1996; Virot et al., 2008,).
    [0006]
    [0007] D-limonene (1-methyl-4- (1-methylethenyl) cyclohexane) is the most common monocyclic monoterpene in nature. It is an important component in various citrus oils (orange, lemon, tangerine, lime and grapefruit) and can reach a concentration in them of 95-98%. Additionally, D-limonene is listed in the Code of Federal Regulations recognized as safe (GRAS) as a flavoring agent and can be found in common foods such as fruit juices, soft drinks, baked goods, ice cream, and puddings.
    [0008]
    [0009] Some products generated in the oxidation of Limonene and combined with surfactants such as APSA-80, have been shown to be effective as repellents and / or deterrents for mosquitoes and mealybugs. However, it is complex for Limonene to mix well, thus avoiding stain / droplet formation and good homogenization (Hollingsworth, 2005).
    [0010]
    [0011] Some mixtures described in patent WO 03/011054 A2 with synergistic effect used for pest control contain at least two of these ingredients: D-limonene, thyme oil, lemon oil, lilac flower oil ( Syringa sp), Nigella sativa oil, wintergreen oil, Linalol, Tetrahydrolinalol, Vanillin, Isopropyl myristate, Piperonal, Geraniol, Triethyl citrate and / or Methyl salicylate.
    [0012] Different formulations of a natural insecticide containing 1-20% by weight of D-Limonene, 1-25% by weight of a non-toxic emulsifying agent (Alkamuls EL 620) and a 55 are described in US Patent 8,133,921 B2. -98% by weight of a non-toxic hydrophilic solvent (depending on the formulation) with effect on ants, aphids, mealybugs, whiteflies, spiders, cicadas, lice, defoliating beetles and their larvae and cockroaches.
    [0013]
    [0014] Components such as Allyl Isothiocyanate, (E) -Nerolidol, Limonene, p-Cymene and y-Terpinene extracted from Eucalyptus globulus show strong larvicidal activity against Aedes aegypti Linn. (Park et al., 2011).
    [0015]
    [0016] In other studies, compositions of essential oils extracted from Eucalyptus tereticornis with a repellent and insecticidal effect and containing monoterpenes such as Mircenol, Citronellic Acid, P-Mentane-3,8-diol, Citronelol, Citronelal and 2,2-dimethyl-5 - (1-Methylethyl) -tetrahydrofuran have been tested on Drosophila melanogaster in bean crops (Murillo-Arango et al. 2014). It was also evaluated whether there was foliar phytotoxicity on the plant, and no such effect was observed.
    [0017]
    [0018] Some limonene-containing formulations such as that described in WO 2011045596 have been used as lepidopteran attractants such as Helicoverpa armígera to be used as a decoy insect and to reduce the number of insect pests in certain crops.
    [0019]
    [0020] In other patents such as WO 2007025197 or WO 2009135289 they focus on the improvement of composition and deterrent and repellent systems against chironomids using elements derived from citrus fruits or from the oxidation of products such as Limonene. The components with such repellent and / or dissuasive capacity that have been observed are Neryl Acetate, Citronellyl Acetate, Geraniol Acetate, Hydroxy-P-Cimeno, Citral, aterpineol, Citronelal, Linalyl Acetate, Citranellol, Terpen-4-ol , Limonene oxidation products such as d- and l-carvone, (+) Limonene oxide, (-) Limonene oxide, cis and trans carveol, diolaldehydes and mixtures of these.
    [0021]
    [0022] The toxicity and repellent effect of pure compounds of plant origin such as Terpineol have been studied on Tribolium confusum (Coleoptera: Tenebrionidae) which is an insect plague of stored cereal products. Neither the repellent effect nor the degree of toxicity of Terpineol were significantly relevant for the control of this pest insect (Ojimelukwe & Adler, 1999)
    [0023] The use of chemical pesticides can cause rapid phytotoxicity problems in plants (leaves, roots and burned flowers) or be taken by it and appear in products intended for human or animal consumption, persisting in the food chain and causing health problems that affect the immune and neurological system (Stella-Nerio et al., 2009)
    [0024]
    [0025] The increase in the problems of synthetic pesticides associated with cross resistance, risks to public health and damage to the environment (accumulating by bioconcentration in the different links of the food chain, in the soil and in the water), have promoted the search of natural products with pesticidal properties. These biopesticides, possess a unique mode of action, are not toxic to humans, plants or animals and act selectively on the species to be eradicated without affecting others. They are low environmental impact products and as they are organic molecules they degrade quickly, avoiding environmental problems of waste accumulation.
    [0026]
    [0027] The present invention advantageously manages to act on harmful insects in agriculture, without involving an increase in environmental residues as it is a product resulting from the synergistic combination in a determined proportion of two products of natural origin, vinegar and essential oil of citrus, in their purified versions of acetic acid and limonene.
    [0028]
    [0029] References
    [0030] WO 03/011054 A2 (Andersch, W .; Wachenhoff-Neuman, U. And Hansler, G. Combination of active agent. Bayer Aktiengesellschaft). 06-26-2000
    [0031] WO 2009135289 A1 (Mullen, B. & Fleming, L. Biological pest control mixture containing d-limonene and nutmeg oil.) 12-11-2009
    [0032]
    [0033] WO 2011045596 A2 (Cork, A. Insect attractant compositions. University of Greenwich) 04-21-2001.
    [0034]
    [0035] US 8,133,921 B2. (McPartland, T. Edible Plant Extract Based Insecticidal Composition) 03-13-2012
    [0036]
    [0037] WO 2007025197 A2 (Deboukian, R.H. & Weldon, P. Spatial inhibitors, deterrents and repellents for mosquitoes and midges. Bedoukian Research Inc.) 01-03-2007.
    [0038] Hollingsworth, RG 2005. Limonene, a Citrus Extract, for control of Mealybugs and Scale insects. Journal of Economic Entomology, 98 (3): 772-779.
    [0039] Murillo-Arango, W .; Araque Marín, P .; Henao-Murillo, B .; Peláez-Jaramillo, CA Insecticide activity of oil / water emulsion of Eucalyptus tereticornis essential oil. http://www.bvs.sld.cu/revistas/pla/vol 18_1_13 / pla13113.htm.
    [0040]
    [0041] Ojimelukwe, PC & Adler, C. 1999. Potential of Zimtaldehyde, 4-Allyl-anisol, Linalool, Terpineol and other Phytochemicals for the Control of the Confused Flour Beetle (Tribolium confusum J. d. V.) (Col., Tenebrionidae) . AnzeJgerfi r Sch idlingskunde Journal of Pest Science, 72: 81-86.
    [0042]
    [0043] Park, HM; Kim, J .; Chang, KS; Kim, BS; Yang, YJ; Kim, GH; Shin, SC & Park, KIL 2011. Larvicidal Activity of Myrtaceae Essential Oils and Their Components against Aedes aegypti, Acute Toxicity on Daphnia magna, and Aqueous Residue. Journal of MedicalEntomology, 48 (2): 405-410.
    [0044]
    [0045] Stashenko, EE; Doors, MA; Combariza & MY 1996. Volatile secondary metabolites from Spilanthes Americana obtained by simultaneous steam distillation-solvent extraction and supercritical fluid extraction. Journal of Chromatography A, (752): 223-232.
    [0046]
    [0047] Stella Nerio, L .; Olivero-Verbel, J & Stashenko, EE 2009. Repellent activity of essential oils: A review. Bioresource Technology, 101 (2010): 372-378.
    [0048]
    [0049] Virot, V., Tomao, V., Giniers, C., Visinoni, F., & Chemat, F. 2008. Green procedure with a green solvent for fats and oils determination. Microwave integrated soxhlet using limonene followed by microwave Clevenger distillation. Journal of Chromatography A, (1196): 147-152.
    [0050]
    [0051] Detailed description of the invention
    [0052]
    [0053] The formulation of a product of organic origin consisting of
    [0054] Limonene (40-70%) and Acetic Acid (60-30%). The combination of both components
    [0055] produces a synergistic effect that gives the product a significant insecticidal capacity
    [0056] on pests in crops that are not obtained using the components separately,
    [0057] therefore, a synergistic action between the two substances is responsible for the efficacy
    [0058] of the present invention. Furthermore, this synergistic action is effective only in a
    [0059] specific margin of the limonene / acetic ratio and outside this range does not work with the
    [0060] same effectiveness.
    [0061]
    [0062] In addition, the invention is illustrated below by means of the
    [0063] corresponding examples.
    [0064] Brief description of the figures
    [0065] Figure 1 . Evolution of the aphid level per leaf in pepper culture under the treatments tested. The thick arrows in the direction of the abscissa axis indicate the day of treatment. The thinner arrows next to the references to the treatments indicate to which line the evolution of the accompanying treatment corresponds.
    [0066]
    [0067] Figure 2 . Evolution of the whitefly population in pepper cultivation for different treatments. The thick arrows in the direction of the abscissa axis indicate the day of treatment. The thinner arrows next to the references to the treatments indicate to which line the evolution of the accompanying treatment corresponds.
    [0068]
    [0069] Preferred embodiments of the invention
    [0070]
    [0071] The present invention is further illustrated by the following 2 examples, which are not intended to be limiting in scope.
    [0072]
    [0073] The product is prepared from the following compounds:
    [0074]
    [0075] -Acetic Acid with a purity of 99.7%, is added in a percentage of 30-60%.
    [0076]
    [0077] -Limene with a purity of 92-99% is added at a percentage of 70-40%.
    [0078]
    [0079] For the elaboration of the mixture, the order when adding the components is acetic acid first, followed by limonene. It is necessary to stir said mixture. The generated product is soluble in water.
    [0080]
    [0081] The application of the synergistic mixture is carried out by means of foliar spraying on the foliar mass of the crop under treatment, previously carrying out a combination of the synergistic mixture with water in the spray tank. The function of water is to act as a dispersion vehicle and to guarantee a homogeneous distribution of the synergistic mixture over the entire surface to be treated.
    [0082]
    [0083] The percentage or dose of the mixture and the amount of application water is variable and will depend on the total leaf area of the crop to be treated (so that the dispersion is maximum) and on applying a dose of the synergistic mixture sufficient to guarantee the insecticidal efficacy of the treatment. It is for this reason that the percentages of synergistic mixing in Treatment broths are carried out at 1 ppm, this concentration being merely indicative and not intended to be limiting in its use, since use at other concentrations may be effective.
    [0084]
    [0085] Example 1
    [0086]
    [0087] The evaluation of the effect of the product formulated with limonene was carried out on a greenhouse scale to determine the influence on aphids. The study was carried out during the months of December 2014 and January 2015 in a greenhouse in full production with organic cultivation of pepper of the 141 Rijkzman variety.
    [0088]
    [0089] The irrigation system is drip and at the time of the test the presence of aphids with very high population levels is observed. The surface of the greenhouse is 9000 m2 and the pepper plants are located within a 0.4 m x 1 m plantation frame.
    [0090]
    [0091] The pepper plants were treated with four different theses: water (as a negative blank), limonene 94%, acetic acid 99.7% and finally, a product formulated with limonene and acetic acid (60:40). With each of these products, the treatment was carried out on the pepper plants by means of a manual spraying equipment at 20 bar pressure.
    [0092]
    [0093] The concentration of the products used was 1 ppm (0.1%) and 40 plants were treated per treatment. A pest level count was performed prior to application to subsequently determine the reduction of insects in them.
    [0094]
    [0095] The counts were made 24 and 72 hours after application, evaluating the mortality of insects present in the leaves and a treatment was again carried out with each of the products. The results of the counts are shown in Figure 1 where the days on which the treatments were applied are marked with an arrow.
    [0096]
    [0097] The average number of aphids observed on the days of application of the products is prior to said treatment.
    [0098]
    [0099] For this, four random treatments were established, which are detailed in Table 2:
    [0100]
    [0101]
    [0102] The different treatments were applied weekly for 2 weeks, making 4 replicates per treatment and establishing plots of 10 pepper plants where aphid counts were made on leaves (10 per plot) prior to treatment, at 24 and 72 hours.
    [0103]
    [0104] Analyzing the results of the study, we observe that T4 remains below the rest of the treatments since the counts of individuals begin after the first day of treatment. As evidenced by the trend line for this treatment, the decrease in the number of aphids per leaf is gradual and constant during the evolution of the trial.
    [0105]
    [0106] Control is maintained above all other treatments as expected, while T2 and T3 follow a very similar trend without exercising control over the aphid infestation, therefore it is concluded that the components of the mixture separately do not have a significant effect on the pest, with T4 being the most effective treatment for its management (figure 1).
    [0107]
    [0108] Example 2
    [0109]
    [0110] The objective of this test is to analyze the effectiveness of the product on whiteflies in different formulations to know the effectiveness of the mixture.
    [0111]
    [0112] The plot under test has an area of approximately 3,000 m2 planted in complete and paired rows, with a planting frame of 1 x 0.5 m of the California pepper variety in production phase.
    [0113] Its irrigation system is drip and has a moderate infestation of pests that
    [0114] they are appropriate for the realization of this experience.
    [0115]
    [0116] Four treatments were evaluated using a statistical design in random blocks of 2
    [0117] x 7 m with 45 plants per test plot and 4 repetitions of each treatment therefore
    [0118] 180 plants per treatment were analyzed.
    [0119]
    [0120] No type of wetting agent or pH regulator was added in the broths made
    [0121] for each of the treatments. A single application was made with a machine
    [0122] manual sprayer at 20 bar pressure and a total of 3 applications for each
    [0123] treatment.
    [0124]
    [0125] The products used and the dose used in the test are those shown in
    [0126] the following table:
    [0127]
    [0128] Table 2 . Doses used in the different treatments for this trial.
    [0129]
    [0130]
    [0131]
    [0132]
    [0133] For the counts, plants were taken at random and the leaves were observed, both the upper and lower sides. Counts were performed the same day before treatment, after 24 hours and after 72 hours.
    [0134]
    [0135] Regarding the results for the whitefly (figure 2), we verified that the plants treated with T-1 decreased their presence at the time of application, but days later they increased their presence again, being the initial and final percentage after all the almost the same or even larger trial.
    [0136]
    [0137] With the T-2 test, it initially follows the same process as with the T-1, but at the end of the test, the percentage of whiteflies has not increased as strongly.
    [0138] In the case of T-3, the fly population continues its growth without apparently affecting the treatments (Figure 2).
    [0139]
    [0140] In the case of treatment T4, a constant decrease in the number of whitefly individuals is verified until its practical disappearance.
    [0141]
    [0142] The presence of auxiliary fauna such as bees and ladybugs is not damaged by treatments T-2, T-3 and T-4.
    权利要求:
    Claims (1)
    [0001]
    1 - Preparation characterized in that it consists of a combination by weight of limonene from citrus extracts and acetic acid from vinegars
    2 - Insecticide characterized in that it comprises a preparation according to claim 1
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    同族专利:
    公开号 | 公开日
    ES2749225B2|2021-04-06|
    ES2749225R1|2020-04-03|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US5556881A|1993-06-14|1996-09-17|Grahn Marisi; Margaret R.|Insect repellent|
    US6784211B1|1997-04-30|2004-08-31|Mcpartland Tor|Ant spray containing d-limonene and methods of making and using the same|
    EP1113719A1|1998-09-15|2001-07-11|Ecoval Inc.|Insecticidal composition|
    US20100196520A1|2007-06-18|2010-08-05|Hanan Elraz|Insect repellent formulations|
    法律状态:
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    优先权:
    申请号 | 申请日 | 专利标题
    ES201700146A|ES2749225B2|2017-02-18|2017-02-18|Synergistic insecticidal combination of vinegar and citrus essential oil|ES201700146A| ES2749225B2|2017-02-18|2017-02-18|Synergistic insecticidal combination of vinegar and citrus essential oil|
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