• 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:
    A microencapsulated insecticidal composition containing isopropyl (2E, 4E)-3,7,11-trimethyl-11-methoxy-2,4-dodecadienoate which comprises 45 - 95% by weight of isopropyl (2E, 4E)-3,7,11-trimethyl-11-methoxy-2,4-dodecadienoate as active ingredient, 1 - 15% by weight of butyl hydroxy toluene and 5 - 40% by weight of activated charcoal, in the form of powdery microcapsules having a grain size of 1 - 300 mu m and coated with a hydroxypropyl methyl cellulose phthalate or cellulose acetate phthalate polymer. The advantage of the microencapsulated insecticidal composition according to the present invention resides in the increased stability.
    公开号:SU1535365A3
    申请号:SU833674499
    申请日:1983-12-02
    公开日:1990-01-07
    发明作者:Фекете Пал；Мадьяр Карой；Майер Анна；Келмен Йожеф；Тот Каталин
    申请人:Эдьт Дьедьсерведьесети Дьяр (Инопредприятие)；
    IPC主号:
    专利说明:

    This invention relates to pest control chemicals and may be used in agriculture.
    The purpose of the invention is to increase the photo stabilization of the well-known drug metoprene, isopropyl- (2E.4E) -3,7,1I-trimethyl-11-megoxy-2,4-dodecadienoate. The preparation is suitable for preventing the spread of insects.
    Example 1. Preparation of micronolysaccharide-type methoprene compositions with and without activated plant carbon and comparing their stability.
    A. In 25.0 g of methoprene, 0.25 g of butylgndroxntoluene is dissolved, and then suspended in this solution.
    2.5 g activated charcoal. The suspension thus obtained is dispersed in a solution of 12.5 g of cellulose acetate phthalate and 250 g of a 6X-aqueous sodium hydroxide solution to obtain a droplet size of 1 to 10 µm. The mixture was diluted by adding 375 ml of water and 125 ml of a 20% aqueous solution of sodium sulfate at copper temperature, with continuous stirring. The mixture is diluted with an additional 125 ml of water, then cooled to 0-5 ° C, after which, with constant stirring, 200 ml of a 1.5% citric acid solution are added until pH 3.5-4 is obtained. The mixture is heated to 60 ° C, stirred at this
    SP
    WITH
    sd
    with
    3 joint venture

    CM
    the temperature of about 1 h, re-cooled, filtered and dried. In this way, a black powder consisting of fine granules is obtained.
    B. Repeat the microencapsulation method described in Test A, a solution in 25.0 g of methoprene, 1.25 g of bu-hydroxytoluene, and a suspension.
    2.5 g activated charcoal.
    C. The microencapsulation method described in Test A is carried out in such a way that 3.75 g of butylhydroxytoluene is dissolved in 25.0 g of methoprene and 10 g of activated charcoal is suspended.
    D. The microencapsulation procedure described in Test A is repeated, with a suspension of 0.25 g of butylhydroxytoluene and 1.25 g of activated vegetable carbon in 25.0 g of methoprene.
    E. The microencapsulation method described in Test A is carried out in such a way that 0.25 g of butylhydroxytoluene is suspended in 25.0 g of methoprene. A yellowish fine powder is obtained with an active ingredient content of 65%.
    F. The microencapsulation method described in Test A is carried out
    without adding stabilizers to metoprene. A yellowish fine powder is obtained. The composition of the drugs is given in table.1.
    Data on the stability of microcapsules are given in table 2.
    From the presented data it is clear that the stability of the content of the biologically active substance of microcapsules is ensured only through the combined use of butyloxytoluene and activated carbon, individually no stabilizer is sufficient. From the point of view of avoiding exposure to light, the protective effect of both substances together is better (experience D 90.6%) than their separate application (experience E 26.2%, respectively experience G 31.6%) or the addition of individual applications (57.8% ).
    From tab. 2, it can be seen that the content of the active ingredient microcapsules not containing activated plant carbon is reduced by more than 80% during the period of illumination, whereas in the case of microcapsules c. the composition of the present invention
    five
    0
    0
    five
    a decrease in the content of the active ingredient varies only from 0 to 27%.
    Example 2. Testing the stability during storage and in the field conditions of a methoprene microencapsulated composition containing activated plant carbon.
    Microcapsules containing 5% butylhydroxytoluene and 10% activated vegetable carbon related to the content of methoprene are prepared according to Example 1. A salt mixture containing about 0.02% of methoprene is obtained from the obtained microcapsules using feed salt. The blocks (diameter 16.5 cm, height about 15 cm) are pressed using the appropriate equipment. Salt blocks are stored under normal conditions (temperature 20-30 ° C, relative humidity 40-70%) and in field conditions in July and August on cattle pasture for 6 weeks. The content of methoprene in salt blocks,%:
    Initial content0,023
    After storage for 8 weeks.
    After storage in field conditions for 6 weeks: in the upper layer 0-1 cm of salt block 0,015
    1-3 cm under the top
    layer0,020
    in the inner layer below 3 cm 0.021 Average content0, 0205 Thus, the content of methoprene in salt blocks containing stabilized microcapsules of methoprene does not decrease during 8-week storage. However, at 6-week field conditions, the average content of active ingredient reduced to 2% per week, and the opposite of the weekly value of about 20%, as described in the prior art.
    Further stability tests are carried out by using salt blocks containing 0.03% stabilizer.
    Bathing methoprene microcapsules in accordance with experiments A and F of example 1. The results are shown in table 3.
    Thus, when stored in storage for 8 months, a decrease in the content of the active ingredient of the sample of about 217 is observed in the upper layer of the salt block, while inside the salt block the content of methoprene remains unchanged, while the content of the active ingredient of the salt block obtained with microcapsules not containing stabilizers, completely decomposed in the outer layer and reduced to 80% inside the salt block.
    EXAMPLE 3: Tests on the biological activity of microcapsules stabilized in accordance with the invention and containing methoprene are examined on larvae of the species Musca domes tica, and the drip method recommended by the WHO is used.
    To carry out tests from micro capsules C, the products of example, experiments A and B), by extraction with ethyl alcohol, obtain a solution containing 0.4% methoprene, which is diluted by an additional twofold dilution to a concentration of 0.2-0,0003%.
    Then, on the larvae in each case 25 flies, found in the third stage, are dripped with 2 ml of the basic solution and obtained in each case after diluting the solution, the application being produced using a Hamilton microdosing device. 25 fly larvae applied to each concentration are placed in a plastic cup. And in each glass previously placed on 20 g of the nutrient medium. In these glasses, the larvae evolve before they are molded.
    A solution of the biologically active substance methoprene in a series of two-fold dilutions is used as a compared solution.
    In the control experiment, the larvae, by analogy with the described process, are treated with absolute alcohol, which does not contain methoprene. The cups are covered with gauze and kept in a thermostat at 30 ° C (2-3 weeks) until the larvae pupate, viable individuals develop from pupae and then die due to lack of water.
    ten
    353656
    Then the gauze is removed, in the glass, the crawled individuals and the dead pupae are counted. Each study is carried out in parallel two times, the results are added, from the joint data the mortality of the pupae is calculated:
    Number of dead pupae d 100
    Mortality of pupae, TL
    The number of dead pupae + the number of crawled individuals
    15
    20
    25 30
    50
    (Mortality in the control experiment is taken into account by the Abbot formula).
    Concentration-related mortality data of the pupae are processed by the transformation method, the LC 50 is determined with a confidence interval relating to the 5% significance level, as well as the LC. The data obtained are presented in Table 4, where the LCSO and are the values, and in the case of these studies, meaning the concentration of methoprene, which, when applied in each case 2 ml of the solution from the larvae of the flies, causes 50% or 90% of the mortality of the pupae.
    In various ways, studies have shown that there is no difference between the biological activity of the initial biologically active substance and the activity of the microencapsulated preparation containing stabilizers.
    权利要求:
    Claims (2)
    [1]
    Invention Formula
    A microcapsule containing a core on the basis of nzopropyl- (2E, 4E) -3,7,11-trimethyl-11-methoxy-2,4-dodecadienoate and a polymer shell, characterized in that, in order to increase the photostability of the active substance, The core additionally contains d5 2,6-di-tert-butyl-4-methylphenol and activated carbon in the following ratio, wt.%:
    Isopropyl- (2E, 4E) -3, 7,11-trimethyl-11-methoxy-2, 4 dodecadienoate 64.5-94.34
    2,6-Di-tert-butyl-4-methylphenol0, 90-9.70
    Activated
    coal 4,72-25,80
    and the shell is made of acetylcellulose phthalate at a mass ratio of the active substance: the shell is 2: 1.
    35
    40
    five
    Table 1
    Note. The ratio of wall material: methoprene in all cases
    is 1:
    [2]
    2. To obtain microcapsules according to the invention, medical activated carbon is used: particle size is more than 40-30%, less than 10 - no more than 20%, specific surface area is 1000-1500 mg / g.
    Table 2
    Storage method
    Initial sample After storage in the warehouse for 8 months: in the upper 0-1 cm layer
    in the inner layer of the salt block
    a b and c a 3
    Content of metoprene,%, according to experience
    ZZTEZ
    0,0300,032
    0.020 Below 0.001
    0.030 0.007

    15.4 24.2
    16.3 14.7
    23.8 25.1
    9.6 85.1
    10.1 86.2
    8.6 83.7
    -f-
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    同族专利:
    公开号 | 公开日
    US4774090A|1988-09-27|
    GB8332218D0|1984-01-11|
    CH658365A5|1986-11-14|
    AT385394B|1988-03-25|
    HU186056B|1985-05-28|
    ATA901783A|1987-09-15|
    GB2128092A|1984-04-26|
    GB2128092B|1985-11-06|
    WO1983003521A1|1983-10-27|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US3912815A|1972-06-09|1975-10-14|Zoecon Corp|Certain 2,4-dienoic acid esters as insect control agents|
    US3904662A|1972-02-07|1975-09-09|Zoecon Corp|2,4-dienoic acids, esters and derivatives|ZA903739B|1989-05-27|1991-03-27|Sumitomo Chemical Co|A poison bait for control of noxious insects|
    DE4330991A1|1993-09-13|1995-03-16|Peter Pelz|Method and device or means for administration of medicinal or health-promoting agents to animals|
    US5846554A|1993-11-15|1998-12-08|Zeneca Limited|Microcapsules containing suspensions of biologically active compounds and ultraviolet protectant|
    US6015570A|1993-12-23|2000-01-18|Tucci Associates, Inc.|Slow-release insect-repellent compositions and uses|
    RU2354699C2|2003-02-03|2009-05-10|ЭШЛЭНД ЛАЙСЕНСИНГ ЭНД ИНТЕЛЛЕКЧУАЛ ПРОПЕРТИ ЭлЭлСи|Composition of coating for food product packing material|
    US7204994B2|2003-02-03|2007-04-17|Ashland Licensing And Intellectual Property Llc|Juvenile hormone compositions and methods for making same|
    WO2005053409A1|2003-12-02|2005-06-16|EGIS Gyógyszergyár Rt.|Insecticidal premix and process for the preparation thereof|
    US7238365B1|2005-02-08|2007-07-03|Wellmark International|Pesticide formulation|
    US7892571B2|2005-02-23|2011-02-22|Wellmark International|Controlled release of S-methoprene and other active ingredients with activated carbon|
    US10645931B2|2016-12-15|2020-05-12|Wellmark International|Extended release formulation|
    US10743535B2|2017-08-18|2020-08-18|H&K Solutions Llc|Insecticide for flight-capable pests|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    HU821042A|HU186056B|1982-04-06|1982-04-06|Insecticide preparate consisting of /2e-4e/-3,7,11-trimetil-11-metoxi-2,4-dodecaidienacid-propilesther|
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