CN1328961C - Sand land cypress micro emulsion and its manufacturing method - Google Patents
Sand land cypress micro emulsion and its manufacturing method Download PDFInfo
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- CN1328961C CN1328961C CNB2003101222311A CN200310122231A CN1328961C CN 1328961 C CN1328961 C CN 1328961C CN B2003101222311 A CNB2003101222311 A CN B2003101222311A CN 200310122231 A CN200310122231 A CN 200310122231A CN 1328961 C CN1328961 C CN 1328961C
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- sandy ground
- cypress
- ground cypress
- podophyllotoxin
- sandy
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Abstract
The present invention relates to a sandy cypress micro-emulsion and a manufacturing method thereof. The preparation form of the micro-emulsion has good environmental compatibility so as to completely exert the advantages of sandy cypress pesticides in the form of high pest eliminating efficiency, no damage to people and livestock and low environmental influence. The present invention comprises the following components: sandy cypress extract with podophyllotoxin, an emulsifying agent, an antifreezing agent and water. The manufacturing method comprises the following operation steps: adding the emulsifying agent to the sandy cypress extract, and then adding the antifreezing agent and the water under a condition of high-speed stirring at room temperature; uniformly stirring; uninterruptedly stirring, heating to the temperature of 70 to 80 DEG C, and then obtaining the sandy cypress micro-emulsion under a state that the paste system is converted to O/W type from W/O type.
Description
One, technical field:
The present invention relates to a kind of insecticide, especially relating to a kind of is the sandy ground cypress microemulsion and the manufacture method thereof of active ingredient with the podophyllotoxin in the sandy ground cypress extract.
Two, background technology:
Nuisanceless Pesticide Research Service Center, Xibei Agroforestry Science and T, found the biologically active of sandy ground cypress first in nineteen ninety, and sandy ground cypress insecticidal activity carried out system research research, on the basis of this research, applied for " " Shadibai " pesticide and manufacture method thereof ", and license, the patent No.: ZL94105885.9 have been obtained.By further research to sandy ground cypress insecticide active substance, three sharp monomeric compounds have therefrom been isolated, the structure assay certificate, these three kinds of compounds are respectively podophyllotoxin, deoxidation podophyllotoxin and β-podophyllotoxin, and have determined that podophyllotoxin is the main active ingredient in the sandy ground cypress.
Carried out further research by structure and activity relationship to podophyllotoxin, podophyllotoxin is modified synthetic gained analog, carry out biologicall test, podophyllotoxin structure and active relation have been drawn, apply for and obtained patent of invention " bactericidal compound and uses thereof ", patent No. ZL02114480.X on this basis; Applied for patent of invention " podophyllotoxin series derivates and application thereof ", application number 200310105870.7.
The sandy ground cypress is a kind of good pesticide plant, and is little to environmental influence to people, animal safety to pest efficient, poor as the Environmental compatibility of its preparation form, can not embody the advantage of " Shadibai " pesticide fully.At present, the development trend of pesticidal preparations is water baseization, solidification, and microemulsion is as a kind of water base chemical preparation, extensive use in each pesticide species.
Three, summary of the invention:
The present invention provides a kind of sandy ground cypress microemulsion and manufacture method thereof in order to solve the weak point in the above-mentioned background technology, and the Environmental compatibility of its preparation form is good, can embody the advantage of " Shadibai " pesticide fully, to pest efficient,, little to environmental influence to people, animal safety.
For achieving the above object, the technical solution used in the present invention is:
A kind of sandy ground cypress pest killing micro emulsion, its special character is to comprise following component: the sandy ground cypress extract, emulsifier, antifreeze and the water that contain podophyllotoxin.
The shared mass percent of above-mentioned each component can be:
The sandy ground cypress extract 10～20% that contains podophyllotoxin
Emulsifier 8～20%
Antifreeze 10～30%
Water 30～72%
Mentioned emulsifier can be OP-10 (octyl phenol polyoxy ethyl ether) and DBS-Ca (calcium dodecyl benzene sulfonate), OP-10: DBS-Ca=5: 3.
Above-mentioned antifreeze can be one or more mixtures in dimethyl sulfoxide (DMSO), ethanol, the methyl alcohol.
A kind of manufacture method of sandy ground cypress pest killing micro emulsion, its special character is to comprise following operating procedure: under the room temperature condition, add emulsifier in sandy ground cypress extract, add antifreeze and water under the high-speed stirred, stir; Keep stirring, be heated to 70～80 ℃, treat that system is converted into the O/W type from w/o type, make sandy ground cypress pest killing micro emulsion.
Above-mentioned sandy ground cypress extract is to get with 95% ethanol cold soaking sandy ground cypress branches and leaves crushed material, and sandy ground cypress branches and leaves are pulverized, and crosses 60 mesh sieves; Crushed material is with 95% ethanol cold soaking 3 times, and the ratio of each time ethanol and crushed material is 8: 1,5: 1,5: 1; Merge 3 times leachate, the ethanol in the leachate is all steamed, must contain the sandy ground cypress extract of podophyllotoxin about 1.5%.
Compared with prior art, the advantage and the effect that have of the present invention is as follows:
The present invention is a kind of water base chemical preparation, and the Environmental compatibility of its preparation form is good, can embody the advantage of " Shadibai " pesticide fully, and is to pest efficient, to people, animal safety, little to environmental influence.
Four, embodiment:
The preparation of embodiment 1:0.15% podophyllotoxin microemulsion
Take by weighing 10 kilograms of sandy ground cypress extracts (containing podophyllotoxin 1.5%), under high-speed stirred, add 10 kilograms of dimethyl sulfoxide (DMSO)s successively, 14 kilogram of 95% ethanol, 10 kilograms of OP-10,6 kilograms of DBS-Ca and 50 kilograms of deionized waters; After mixing, be heated with stirring to 75 ℃, after system to be stirred is homogeneous liquid, be cooled to room temperature, promptly get 0.15% podophyllotoxin microemulsion.
The preparation of embodiment 2:0.3% podophyllotoxin microemulsion
Take by weighing 20 kilograms of sandy ground cypress extracts (containing podophyllotoxin 1.5%), under high-speed stirred, add 12 kilograms of dimethyl sulfoxide (DMSO)s successively, 12 kilogram of 95% ethanol, 12.5 kilograms of OP-10,7.5 kilograms of DBS-Ca and 48 kilograms of deionized waters; After mixing, be heated with stirring to 75 ℃, after system to be stirred is homogeneous liquid, be cooled to room temperature, promptly get 0.3% podophyllotoxin microemulsion.
Test 1: preparation stability test
The stability of emulsion test
Get 1ml0.15% podophyllotoxin microemulsion and add in the 200ml 342mg/L standard hard water, under 30 ℃, leave standstill 30min,
Emulsion keeps pellucidity not have grease suspension or solid precipitation, and can mix than row with any with water.
Cold storage stability test
Get 0.15% podophyllotoxin microemulsion 30ml, in the clear, colorless glass port grinding bottle of packing into, sealing is placed on 0 ~-10 ℃ of refrigerator and cooled and hides, and takes out to place under the room temperature behind the 24h and observes, and preparation recovers transparent by caking, repeated multiple times, good reproducibility.
The heat storage stability test
Preparation is packed in the ampoule bottle, place under 54 ± 2 ℃ of conditions and stored for 2 weeks, detecting the average resolution ratio of podophyllotoxin is 1.2%,
The preparation outward appearance keeps homogeneous phase transparent.
The analysis of effective component method
Adopt the content of high-efficient liquid phase chromatogram technique analysis active ingredient podophyllotoxin.Chromatographic condition is:
Chromatographic column: C
18Post; Detector: diode array detector; Detect wavelength: 218nm; Flowing phase: methyl alcohol+water=65+35 (V/V); Flow velocity: 1ml/min: sampling volume: 5 μ l; Quantitative approach: external standard method.
The biologicall test of test 2:0.15% podophyllotoxin microemulsion
With 400,800,1200,1600,2000 times of 0.15% podophyllotoxin microemulsion dilutions, and establish the clear water contrast.Gather
Fresh cabbage leaves is cut into the vanelets of 2cm * 2cm, and the blade that shears was immersed in the good soup of dilution 5 seconds, and taking-up is dried, put into diamond-back moth and give birth to and survey special box, then each give birth to survey insert in box 3 age 10 of diamondback moth larvaes, every processing repeats 3 times.Inspection in 72 hours borer population alive behind the medicine, the calculation correction lethality.It is 98% that 72 hours corrected mortalities of diamond-back moth are handled in 0.15% podophyllotoxin microemulsion dilution 400; It is 86% that 72 hours corrected mortalities of diamond-back moth are handled in 0.15% podophyllotoxin microemulsion dilution 800; It is 75% that 72 hours corrected mortalities of diamond-back moth are handled in 0.15% podophyllotoxin microemulsion dilution 1200; 0.15% podophyllotoxin microemulsion dilution 1600; Handling 72 hours corrected mortalities of diamond-back moth is 58%; It is 40% that 72 hours corrected mortalities of diamond-back moth are handled in 0.15% podophyllotoxin microemulsion dilution 2000.
Test 3:0.3% podophyllotoxin microemulsion field medicine effect test
Giving birth to the pesticide field efficacy medicine test criterion of surveying the chamber formulation with reference to The Institute for the Control of Agrochemicals of the Ministry of Agriculture,PRC carries out.
Reagent agent: 0.3% podophyllotoxin microemulsion
10% permethrin milk oil (Jiangsu Chemical Pesticide Group Co. Ltd)
For studying thing and controlling object: wild cabbage, diamond-back moth
Test procedure: experimental field be located at vegetable plot, Yangling District Li Tai township, establish 500,1000 and 1500 times of three concentration of 0.3% podophyllotoxin microemulsion, 2000 times of 10% permethrin milk oils, clear water is contrast, totally five processing.4 repetitions are established in every processing, totally 20 sub-districts.Sub-district area 20m
2, district's group is arranged at random.Medicament is diluted to desired concn, carries out conventional spray with workers and peasants-16 type knapsack hand sprayer then, mu spouting liquid 50kg/ mu, evenly spray is distributed in the blade tow sides.Decide 5 points in every sub-district with 5 point samplings before the dispenser, decide 2 of wild cabbages, the mark of listing at every.The insect population radix of investigation diamond-back moth before the dispenser.Behind the spray medicine 1,3,7d investigates remaining borer population alive on the wild cabbage of mark, the insect population that calculates each treatment region go down rate and preventive effect (the results are shown in Table 1).
Table 1 0.3% podophyllotoxin microemulsion control diamond-back moth result of the test
| Handle | The average preventive effect of 1d (%) behind the medicine | The average preventive effect of 3d (%) behind the medicine | The average preventive effect of 7d (%) behind the medicine |
| 500 times of 0.3% podophyllotoxins | 27.9 | 89.2 | 93.6 |
| 1000 times of 0.3% podophyllotoxins | 19.0 | 76.5 | 84.5 |
| 1500 times of 0.3% podophyllotoxins | 11.7 | 66.1 | 77.7 |
| 2000 times of 10% permethrin milk oils | 63.4 | 85.3 | 92.1 |
Claims (4)
1, a kind of sandy ground cypress pest killing micro emulsion, it is characterized in that comprising following component: the sandy ground cypress extract, emulsifier, antifreeze and the water that contain podophyllotoxin, the shared mass percent of each component is: the sandy ground cypress extract 10～20% that contains podophyllotoxin, emulsifier 8～20%, antifreeze 10～30%, water 30～72%, wherein emulsifier is OP-10 and DBS-Ca, antifreeze is dimethyl sulfoxide (DMSO) and methanol mixture.
2, a kind of sandy ground cypress pest killing micro emulsion according to claim 1 is characterized in that: OP-10 in the described emulsifier: DBS-Ca=5: 3.
3, a kind of manufacture method of sandy ground cypress pest killing micro emulsion, it is characterized in that comprising following operating procedure: under the room temperature condition, the adding mass percent is 8～20% emulsifier op-10 and DBS-Ca in sandy ground cypress extract, the adding mass percent is 10～30% antifreeze dimethyl sulfoxide (DMSO) and methanol mixture and water under the high-speed stirred, stirs; Keep stirring, be heated to 70～80 ℃, treat that system is converted into the O/W type from w/o type, make sandy ground cypress pest killing micro emulsion.
4, the manufacture method of a kind of sandy ground cypress pest killing micro emulsion according to claim 3, it is characterized in that comprising following operating procedure: described sandy ground cypress extract is to get with 95% ethanol cold soaking sandy ground cypress branches and leaves crushed material, sandy ground cypress branches and leaves are pulverized, crossed 60 mesh sieves; Crushed material is with 95% ethanol cold soaking 3 times, and the ratio of each time ethanol and crushed material is 8: 1,5: 1,5: 1; Merge 3 times leachate, the ethanol in the leachate is all steamed, must contain the sandy ground cypress extract of podophyllotoxin about 1.5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101222311A CN1328961C (en) | 2003-12-30 | 2003-12-30 | Sand land cypress micro emulsion and its manufacturing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101222311A CN1328961C (en) | 2003-12-30 | 2003-12-30 | Sand land cypress micro emulsion and its manufacturing method |
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| Publication Number | Publication Date |
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| CN1555709A CN1555709A (en) | 2004-12-22 |
| CN1328961C true CN1328961C (en) | 2007-08-01 |
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| CNB2003101222311A Expired - Fee Related CN1328961C (en) | 2003-12-30 | 2003-12-30 | Sand land cypress micro emulsion and its manufacturing method |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104510704B (en) * | 2013-09-30 | 2018-04-27 | 中国科学院理化技术研究所 | A kind of male antifertility medicine emulsion and preparation method thereof |
| CN106172384A (en) * | 2016-06-08 | 2016-12-07 | 韩立 | A kind of podophyllotoxin micro-emulsion insecticide |
| CN110301446A (en) * | 2019-07-23 | 2019-10-08 | 泰安市农业科学研究院 | A kind of plant source preparation and preparation method thereof preventing and treating tea tree sucking pest |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1097932A (en) * | 1994-06-01 | 1995-02-01 | 西北农业大学 | " Shadibai " pesticide and manufacture method thereof |
| CN1332165A (en) * | 2001-02-27 | 2002-01-23 | 西北农林科技大学无公害农药研究服务中心 | Podophyllotoxin compound and its application in pesticide |
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2003
- 2003-12-30 CN CNB2003101222311A patent/CN1328961C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1097932A (en) * | 1994-06-01 | 1995-02-01 | 西北农业大学 | " Shadibai " pesticide and manufacture method thereof |
| CN1332165A (en) * | 2001-02-27 | 2002-01-23 | 西北农林科技大学无公害农药研究服务中心 | Podophyllotoxin compound and its application in pesticide |
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