CN1150826C - Application of cnidium fruit extract in preparing agricultural pesticide - Google Patents
Application of cnidium fruit extract in preparing agricultural pesticideInfo
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- CN1150826C CN1150826C CNB011367881A CN01136788A CN1150826C CN 1150826 C CN1150826 C CN 1150826C CN B011367881 A CNB011367881 A CN B011367881A CN 01136788 A CN01136788 A CN 01136788A CN 1150826 C CN1150826 C CN 1150826C
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- ethyl acetate
- frutus cnidii
- osthole
- insecticide
- cnidium fruit
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Abstract
The present invention relates to the application of common cnidium fruit extract on the production of agricultural insecticide. Botanical pesticide which is prepared from the common cnidium fruit extract of the present invention has better touch kill effect on various pests, such as cabbage white butterflies, tea geometrids, cotton bollworms, beet noctuids, rice leaf rollers, henosepilachna vigintioctopunetatas, colcaphellusbowringis and aphids, and the botanical pesticide is safe to people, livestock and other mammals. When the common cnidium fruit extract of the present invention is compounded and matched with various kinds of biotic pesticide and/or chemical pesticide, obvious synergy is generated.
Description
The present invention relates to the purposes of common cnidium fruit P.E in the agricultural chemicals preparation.
Cnidium monnieri Cnidium monnieri (L) Cuss is a samphire, annual herb.Stem is upright, and is cylindrical, high 30～80 centimetres, and vertical rib is arranged, and dredges and gives birth to fine and soft hair.The root leave has handle, and blade is avette, and 2-3 returns pinnation, final sliver wire lanceolar, and tip is sharp-pointed.The blade on stem top is similar to the root leave, but petiole is shorter.Universal umbel top elder generation or adnation.10～25 on umbrella stalk, 8～10 of base portion phyllarys, linear, the tool echinid; 8～10 of involucel sheets, linear; The calyx tooth is not obvious, petal white, 5 lobes, obovate; 5 pieces on stamen, with the petal alternate, filigree is elongated, the flower pesticide ellipse; Ovary is the next, 2 pieces of styles, style base portion taper shape.The diachenium ellipse, the fruit rib becomes aliform, does not have hair.Be born in hillside thick grass, the field.All there is distribution in the most of area of China.
The fruit of cnidium monnieri is called frutus cnidii, different name snake rice, snake grain, snake pearl, wild fennel, toothed habenaria root, favus-infected head beggar.The hot cool and numb tongue of frutus cnidii flavor, its effect of warming kidney and strengthening yang is very sure, so this medicinal material is usually used in treating impotence.Though the anti-woman vagina trichomonad effect of common cnidium fruit P.E there is the report of the pros and cons, but still have in many woman vagina topical agents frutus cnidii as important or main medicine simply, promptly utilize frutus cnidii treatment trichomonas vaginitis, women's pruritus vulvae, eczema of vulva.These medicaments comprise JIEERYIN XIYE (Chengdu En Wei pharmaceutical Co. Ltd), FUYINJIE (Yuantang Pharmaceutical Factory, Guangxi) etc.Although frutus cnidii has certain insecticidal and antibacterial activity, do not find common cnidium fruit P.E is used to prepare the report of agricultural chemicals so far.
The purpose of this invention is to provide the purposes of common cnidium fruit P.E on agricultural insecticide is produced, just common cnidium fruit P.E is used to prepare agricultural chemicals.
The inventor finds that in the screening process of pollution-free plant source pesticide common cnidium fruit P.E itself has certain activity of killing the various agricultural insect.If with the plant extracts of itself and other kind,, can form a series of agricultural insecticides preferably as suitable compatibility such as Thunder God boisiana extract, shrubby sophora extract, seal chinaberry or China tree extract, Lignum cinnamomi camphorae extract, Celastrus angulatus extract, Azalea pontica extract.If with the biopesticide of itself and other kind, composite by a certain percentage as Avermectin, bacillus thuringiensis, can produce obvious synergistic effect, form the public nuisance-free agricultural chemicals of a series of safety and low toxicity, be applicable to the production of pollution-free food.If with itself and some conventional chemosynthesis insecticides, composite by a certain percentage as Methomyl, decis, beta-cypermethrin or the like, also show obvious synergistic effect, can play the lifting insecticidal effect, reduce the effect of chemical pesticide consumption.
The inventor goes through the several years and has studied the insecticidal activity of common cnidium fruit P.E to the variety classes insect, frutus cnidii and of the synergistic effect of different plant extracts compatibilities have been inquired into to insecticidal activity, screened the optimum compound proportion example of Osthole with different agriculture chemical compoundings, having carried out with Osthole according to the relevant rules of national agricultural chemicals management simultaneously is the safety evaluatio and the field efficacy evaluation of the agricultural insecticide of main insecticidal activity component, developed that to have the speed of knocking down fast, insecticidal spectrum is wide, the non-harmful Osthole series of safety and low toxicity agricultural insecticide, thus the present invention finished.
A. the preparation method of common cnidium fruit P.E
Common cnidium fruit P.E of the present invention (this paper is called the frutus cnidii insecticide mother liquor again) prepares in order to the below method:
After air-dry frutus cnidii pulverizing, with the ethyl acetate extracting of heat, concentrating under reduced pressure behind the cracklings removal; Perhaps
After air-dry frutus cnidii pulverizing, with ethanol, methyl alcohol, acetone, chloroform or benzinum extracting, concentrating under reduced pressure behind the cracklings removal; Perhaps
The Common Cnidium Fruit that is crushed to suitable fineness is packed in the empty ion exchange column, soaks, make the extracting that refluxes repeatedly of solvent ethyl acetate with ethyl acetate, concentrate contain insecticide active substance extract to thick; Perhaps
The Common Cnidium Fruit that is crushed to suitable fineness is packed in the empty ion exchange column, soaks, make the extracting that refluxes repeatedly of solvent methanol, ethanol, acetone or chloroform with methyl alcohol, ethanol, acetone or chloroform, concentrate contain insecticide active substance ethyl acetate solution to thick.
All contain Osthole in the common cnidium fruit P.E of the present invention.
Below be the detailed preparation method of common cnidium fruit P.E of the present invention (frutus cnidii insecticide mother liquor):
A-1. the hot extraction process of ethyl acetate
Air-dry good frutus cnidii is broken into Powdered with beater disintegrating machine, crosses 40～100 mesh sieves.It is an amount of to add ethyl acetate in one-level lixiviate jar (chuck or tubulation that heating usefulness is arranged), feeds steam while stirring in chuck, makes ethyl acetate be preheating to 45 ℃-65 ℃.(the frutus cnidii powder: ethyl acetate, ratio W/V) adds Common Cnidium Fruit in the lixiviate jar to press 1: 4～6.Keep the material temperature at 50 ℃～65 ℃ in the leaching process, the lixiviate overall process does not stop to stir all the time.Extraction time is more than 6 hours.By plate and frame filter press, leach the ethyl acetate that contains active substance, collect standby.Filter residue is packed in the secondary lixiviate jar, according to said process, uses fresh ethyl acetate solution again, and extracting one time is so that come out the abundant lixiviate of the insecticide active substance in the Common Cnidium Fruit.After plate and frame filter press, collect filtrate, discard filter residue.The ethyl acetate solution that merges secondary lixiviate gained concentrates 10～40 times by vacuum concentrator with extract, is frutus cnidii insecticide mother liquor of the present invention.
A-2. the hot extraction process of ethanol
50 ℃-65 ℃ of ethanol temperature, and ethanol consumption 1: 4～5 (the frutus cnidii powder: ethanol, W/V), extraction time 6-12 hour, do not stop in the leaching process to stir.Leach the ethanolic solution that contains insecticide active substances such as Osthole by plate and frame filter press, collect standby.Filter residue reinstalls in another lixiviate jar, the fresh ethanol of in the lixiviate jar, packing into according to the above ratio, and carry out second time extracting by above-mentioned way.For guarantee that insecticide active substance is fully extracted from raw material, need repeat above-mentioned extractive process three times.The ethanolic solution that merges first, second time extracting and get by vacuum concentrator with its concentrated 20-60 doubly, promptly gets the said frutus cnidii insecticide mother liquor of the present invention.The ethanolic solution of the 3rd time extracting gained is used for the first pass extracting of the fresh frutus cnidii powder of next group as solvent.
A-3. the hot extraction process of methyl alcohol, acetone, chloroform and benzinum
The same A-2 of leach extraction method, ethanol that only will be wherein changes the methyl alcohol (perhaps acetone, chloroform) of heat into or near the hot benzinum of boiling point.
A-4. cold-draw formulation
Be ready to one of ion exchange column (stainless steel), the ethyl acetate of packing in advance is an amount of, by compressed air the ethyl acetate appropriateness is seethed then, and to add the Common Cnidium Fruit (fineness 40 to 60 orders) that crushes some while seethe.Close the advancing of exchange column, tapping valve, allow Common Cnidium Fruit leave standstill and soaked 1-2 days.Be dipped into wash out insecticide active substance in the Common Cnidium Fruit with the flow velocity of one of per minute one thousandth to two percentage column volume with fresh ethyl acetate after fixing time.Content by Osthole in high pressure liquid chromatography (method is seen embodiment 3) the monitoring eluate when Osthole content is lower than 10 μ g/ml, can stop the process of washing out.Collect the ethyl acetate solution that all contains element, its vacuum concentration is the frutus cnidii insecticide mother liquor for 5～40 times, this extract promptly can be used for pesticide producing.If the Osthole content that soaks in the extract of elution process front surpasses 6000 μ g/ml, then can be directly used in the agricultural chemicals preparation without concentrating.
When cold process is extracted the frutus cnidii insecticide active substance, above-mentioned solvent-ethyl acetate can be changed into organic solvents such as methyl alcohol or ethanol, acetone, chloroform.
B. the preparation method of common cnidium fruit P.E agricultural insecticide list agent
Common cnidium fruit P.E is mixed with one or more insecticides adjuvants, can make the agricultural insecticide of various formulations.
Below be the detailed preparation method of various insecticide list agent:
B-1. Osthole insecticidal emulsifiable concentrate
With above-mentioned frutus cnidii insecticide mother liquor (being common cnidium fruit P.E) with the used solvent of ethyl acetate or other emulsifiable concentrates for agricultural chemicals agent suitably after the dilution, (see Table 1) in proportion and add various insecticides adjuvants and special synergistic agent " 908 ", at last with toluene (or ethyl acetate, dimethylbenzene etc.) constant volume, stir the back.The content range of Osthole can not wait from 0.1%～1.5% in emulsifiable concentrate, generally with 0.3%, 0.4%, 0.6%, 0.8% 4 kind of specification be comparatively suitable.
Table 1 Osthole insecticidal emulsifiable concentrate basic components
| The missible oil raw material | Ratio (%) |
| Frutus cnidii insecticide mother liquor surfactant TX-10 bleeding agent 961 synergist, 908 solvent toluenes (or ethyl acetate, dimethylbenzene etc.) | (actual content by Osthole in the mother liquor calculates definite) 3～15 2.5～12 3～12 is settled to volume required |
B-2. Osthole wettable insecticidal dust
With absorption such as frutus cnidii insecticide mother liquor precipitated calcium carbonate, diatomite, kaolin, add surfactant such as pulp powder again, dodecyl sodium sulfate salt, the withered powder of tea or the like also add dispersant, special synergistic agent and bleeding agent, crushing screening behind the abundant mixing.In frutus cnidii wettable insecticidal dust, the Osthole content range can not wait from 0.2%-2%, generally with 0.6%, 0.8%, 1.2% 3 kind of specification be comparatively suitable.Osthole wettable insecticidal dust basic recipe is as shown in table 2:
Table 2 Osthole wettable insecticidal dust basic recipe
| The pulvis material name | Ratio (%) |
| Frutus cnidii insecticide mother liquor adsorbent (diatomite, kaolin, lightweight CaCO 3) wait the white carbon black of the withered powder synergist of tea " 909 " dispersant (draw back powder, sodium carbonate of lignin, Nongru-700 number etc.) bleeding agent (961, azone etc.) | (pressing the plain actual content calculating of frutus cnidii in the mother liquor) 40～70 2～25 2～10 5～10 2～15 5～20 |
C. the preparation method of frutus cnidii insecticide mother liquor and other agricultural insecticide complex preparation
With common cnidium fruit P.E and one or more other kind plant extracts compatibilities, can make insecticide pesticide; Perhaps
Common cnidium fruit P.E and one or more agricultural insecticides are mixed, can make Recompounded pesticide.
Osthole insecticidal emulsifiable concentrate or Osthole wettable insecticidal dust is composite by proper proportion and Avermectin, bacillus thuringiensis, thunder godvine alkaloid, China tree, melia toosendan, nimbin, matrine etc., and with carbamates, pyrethroid, neires toxin etc. Multiple Pesticides is composite can obtain certain synergistic effect.The frutus cnidii insecticide mother liquor sees Table 3 with the proper ratio scope of different agriculture chemical compoundings.
Table 3 and frutus cnidii pesticide compositional have the suitable compound proportion scope of all kinds of agricultural chemicals of synergistic effect
| Cnidium fruit preparation *(A) | Other agricultural chemicals (title, content) (B) | Compound proportion scope (the A: B) that synergistic effect is arranged |
| 0.4% missible oil | Avermectin 0.9% missible oil Avermectin 0.9% missible oil Avermectin 1.8% missible oil Avermectin 1.8% missible oil | (1～25)∶1 1∶(1～10) (1～13)∶1 1∶(1～5) |
| 0.4% missible oil, 0.6% wetting powder | Bacillus thuringiensis,Bt 2000IU/mg aqueous suspension bacillus thuringiensis,Bt 2000IU/mg aqueous suspension bacillus thuringiensis,Bt 8000IU/mg wetting powder bacillus thuringiensis,Bt 8000IU/mg wetting powder | 1∶(1～12) (1～10)∶1 1∶(1～10) (1～20)∶1 |
| 0.4% missible oil | Beta-cypermethrin 4.5% missible oil beta-cypermethrin 4.5% missible oil | 1∶(1～10) (1～30)∶1 |
| 0.6% wetting powder | Methomyl 90% soluble powder Methomyl 90% soluble powder | 1∶(1～20) (1～50)∶1 |
| 0.6% wetting powder | Chlorophos 90% crystal chlorophos 90% crystal | 1∶(1～20) (1～30)∶1 |
| 0.4% missible oil | Matrine 0.36% missible oil matrine 0.36% missible oil | 1∶(1～30) (1～30)∶1 |
| 0.4% missible oil | Wilforine 0.3% missible oil wilforine 0.3% missible oil | 1∶(1～20) (1～20)∶1 |
| 0.6% wetting powder | Desinsection list 90% wettable powder desinsection list 90% wettable powder | 1∶(1～30) (1～30)∶1 |
Illustrate: Osthole insecticide (A) is an example with the missible oil of 0.4% content and the wetting powder of 0.6% content only in the table 3, the Osthole insecticide of different content equally can with above-mentioned agriculture chemical compounding, final compound proportion can be calculated by Osthole content and draw.In like manner, various insecticides (B) also can be the products with the different content of kind in the table 3, and the optimum compound proportion example also can be calculated by insecticide active substance content and obtain after the change content.
Embodiment 1 hot method is extracted the frutus cnidii insecticide active substance
Extract and use instrument and equipment: beater disintegrating machine, lixiviate jar, plate and frame filter press, boiler, air compressor, vacuum film inspissator, high pressure liquid chromatograph.
Extract required main medicine and reagent: ethyl acetate, methyl alcohol, Osthole standard items.
Leaching process (is example with the double centner frutus cnidii):
A. frutus cnidii is pulverized: air-dry good frutus cnidii is smashed with beater disintegrating machine or multifunctional crusher, crossed 40～100 mesh sieves.Owing to contain Chuck Steak in the frutus cnidii, can be in 1 before pulverizing: (0.5～1) (snake: leaf W/W) ratio be mixed quantitative camphortree leaf powder or root bark of celastrus angulatus powder, promptly adds 50 to double centner camphortree leaf powder or root bark of celastrus angulatus powder.The machine of going up is then pulverized, and can avoid like this because of the oil problems of stopping up sieve aperture more.
B. first pass lixiviate: in 1000 liters of lixiviate jars (stainless steel), quantitatively add 500 liters of ethyl acetates.By the chuck of lixiviate jar, the ethyl acetate temperature is raised to 50 ℃ ± 5 ℃ with steam.Take by weighing the powder after the double centner frutus cnidii is pulverized, drop in the lixiviate jar.Cover tight charging aperture, continue to stir 8 hours, keep the material temperature at 55 ℃-65 ℃.After 8 hours the compressed air of 0.2～0.5Mpa is introduced in the lixiviate jar, utilized air pressure that feed liquid is pressed in the plate and frame filter press.Collect the plain ethyl acetate that contains after filtering, can obtain containing about 415 liters plain ethyl acetate solution usually.
C. second time lixiviate: in 1000 liters of lixiviate jars, quantitatively add 400 liters of ethyl acetates, be preheated to 50 ℃ ± 5 ℃ through jacket steam.Filter residue after the first pass lixiviate is packed in the lixiviate jar into the lixiviate 8～12 hours again of the technological parameter of pressing the first pass leaching process rapidly.Sampling detects the content (method is the HPLC method, sees embodiment 3 for details) of Osthole in the residue after 8 hours, if the content of Cnididin is lower than 100 μ g/g siccative, then lixiviates again in the residue.Through plate compression, collect filtrate, discard filter residue.This time can obtain 380 liters approximately again and contain plain ethyl acetate solution.
D. concentrate: merge the resulting plain ethyl acetate (about 795 liters) that contains of secondary extracting, 50 ℃ ± 5 ℃ vacuum films concentrate.Concentrate about 20 times, make Osthole content in the concentrate 〉=12000 μ g/ml.The recovery ethyl acetate is used for the production of back.Concentrating gained frutus cnidii extract promptly is the mother liquor that foregoing various Osthole insecticide is produced.The double centner frutus cnidii can obtain 40.5 kilograms in above-mentioned mother liquor approximately through extracting and concentrating.
Illustrate: the extraction solvent ethyl acetate in this extracting method can be changed into methyl alcohol (perhaps ethanol, acetone, chloroform and benzinum).Still be higher than 100 μ g/g siccatives if change the content of Osthole in the residue of twice lixiviate behind the solvent, can carry out the 3rd time lixiviate.
Embodiment 2 cold process are extracted the frutus cnidii insecticide active substance
Extract required instrument and equipment: beater disintegrating machine, ion exchange column (stainless steel, void column), 2 head tanks, leaching liquor receiving tank, air compressor, vacuum film inspissator, high pressure liquid chromatograph.
Extract required main medicine and reagent: ethyl acetate, methyl alcohol, Osthole standard items.
Leaching process (is example with the double centner frutus cnidii): a. frutus cnidii is pulverized: method is with embodiment 1, and is more suitable but smashing fineness is controlled at the 40-60 order.B. adorn post: close tapping valve and discharging opening under the post, the 120 liters of ethyl acetates of packing in advance in volume is 200 liters empty ion exchange column drop into 50kg frutus cnidii powder then.Adorn two on post altogether.Open the feed liquor valve of logical head tank 1 (in fresh ethyl acetate is housed), in post, replenish an amount of ethyl acetate.Close feed liquor valve and charge door.C. leave standstill lixiviate: left standstill lixiviate 1～2 day, temperature is that room temperature gets final product.D. cycling elution: open post lower end tapping valve and post upper end feed liquor valve, the control flow velocity is one of per minute three a percentages column volume, closes the valve under the head tank 1 after 400 liters of left and right sides leaching liquors are arranged in the leaching liquor receiving tank, stops to wash post with fresh ethyl acetate.To contain plain ethyl acetate with compressed air and be pressed onto in the head tank 2, carry out cycling elution.The cycling elution process is carried out 2 times and is got final product.E. clean: behind twice of the cycling elution, the fresh ethyl acetate of using instead in the head tank 1 is cleaned, and the control flow velocity is one of per minute five a percentages column volume.After washing 1.5 column volumes, on HPLC, survey the content X of Osthole in the eluent every sampling in 1 hour, if X≤20 μ g/ml then are considered as the insecticide active substance in the cleaned residue.F. concentrate: collect eluent (promptly containing plain ethyl acetate), concentrate about 20 times with the vacuum film inspissator, the frutus cnidii insecticide mother liquor.Every double centner frutus cnidii can get 41 kilograms in mother liquor.
Illustrate: the solvent ethyl acetate can be changed into methyl alcohol (perhaps ethanol, acetone, chloroform) in this extracting method, changing the needed solvent of solvent afterwash step must amount have a certain proportion of increase.
The preparation of embodiment 3 0.4% Osthole insecticidal emulsifiable concentrates
Produce required instrument and equipment: preparing tank, measuring tank, air compressor, automatic packer, high pressure liquid chromatograph.
Produce required main medicine and reagent: frutus cnidii insecticide mother liquor (self-control), ethyl acetate, toluene (or dimethylbenzene), methyl alcohol, TX-10, bleeding agent 961, synergist 908, Osthole standard items.Production process: assay in a. extract: adopt the HPLC method, concrete operation method is seen the last of this section.If Osthole content is 12000 μ g/ml in the measurement result extract.In addition, establish and once make 1000 liters of missible oil.B. weighing: in the ratio of table 1, measure 335 liters of extracts with measuring tank respectively, 200 liters of ethyl acetates, " 961 " 65 liters, take by weighing TX-10 80kg with platform scale, " 908 " 50kg.C. modulation: (titles) sequencing of getting according to quantity, all raw materials are dropped into respectively in the modulation jar, the intact a kind of material of every throwing starts agitator stirring 5～10 minutes immediately.Thrown the final volume (see a jar interior graduation mark) of " 908 " back, started again and stir 60 minutes, promptly become frutus cnidii insecticidal emulsifiable concentrate semi-finished product (volume is 1000 liters) with toluene (or dimethylbenzene) constant volume to 1000 liter.D. product quality inspection: the core index of this product quality inspection is an Osthole content, and its content is controlled to be X 〉=0.4% (W/W).
The method of inspection adopts the HPLC method: the measuring column condition is U.S.'s Beckman high pressure liquid chromatograph, the reverse post of C 18,5 μ m; Two extremely manage array detector, detect wavelength 322nm; Room temperature; Post is pressed 10～12Mpa; Sample size 10 μ l; Flowing phase is methyl alcohol: water=80: 20, flow velocity 1ml/ minute.
Take by weighing 10 milligrams of Osthole standard items earlier, accurately be diluted to 20 μ g/ml, 40 μ g/ml, 60 μ g/ml, 80 μ g/ml, five kinds of concentration of 100 μ g/ml with methyl alcohol.Measure the corresponding peak area (Y) of each concentration (X) respectively, and calculate X, the Y linear regression equation Y=a+bx between the two.Get 1 milliliter of 0.4% Osthole insecticidal emulsifiable concentrate then, in the 100ml volumetric flask, accurately dilute and constant volume with methyl alcohol.Getting 10 μ l behind the mixing advances post and measures its absworption peak area.Repeat for three times, get in the above-mentioned linear regression equation of mean value substitution of the peak area that repeats for three times and obtain corresponding Osthole content x '.Osthole content X=100x ' (μ g/ml) in the semi-finished product missible oil.Product is qualified when X 〉=4000 μ g/ml.E. packing: with automatic filling machine semi-finished product are distributed into 100ml or 250ml bottle, post label and be packaged into case and be 0.4% Osthole insecticidal emulsifiable concentrate product.
0.4% Osthole insecticidal emulsifiable concentrate toxicity test result
Through Tongji Medical Univ's chemistry security assessment centers test, 0.4% Osthole missible oil belongs to low-toxin farm chemicals, meets the pollution-free food production requirement.Concrete outcome is as follows:
1. per os acute toxicity experience: adopt the Wistar rat, female LD
50=3163mg/kg (1878～5326mg/kg), male LD
50=3687mg/kg (2729～4982mg/kg), belong to low toxicity.
2. through the skin acute toxicity experience: adopt the Wistar rat, female, male LD
50All, belong to low toxicity greater than 2000mg/kg.
3. eye irritant test: adopt white rabbit, the result is the moderate excitant.
4. skin irritatin test: adopt white rabbit, the result is slight excitant.
5.Ames test: adopt TA97, TA98, TA100, TA102 four bacterial strains, feminine genders as a result.
6. bone marrow cell micronucleus test: adopt Kunming mouse, the result is negative.
7. testis spermatocyte chromosomal aberration test: adopt Kunming mouse, the result is negative.
8. cumulative toxicity test: adopt adult Wistar rats just, cumulative coefficient is greater than 5, is the slight property accumulated.
0.4% Osthole missible oil the results are shown in Table 4,0.4% Osthole missible oil land for growing field crops insecticidal tests to the toxicity test of difference examination worm and the results are summarized in table 5.
Table 4 0.4% Osthole missible oil is to the Toxicity Determination result of eight kinds of examination worms
*
| The insect title | Worm instar attitude | Toxicity regression formula (Y=aX+b) | In dead, measure or middle concentration *(LC 50) | 95% confidence interval |
| Radish aphid | Nymph | 5.7346X+2.9378 | 2.2888 | 2.26-5.32 |
| Radish aphid | Adult | 3.8606X+1.1808 | 9.7561 | 3.10-16.456 |
| Cotton bollworm | 1 day age | 3.2504X+0.8208 | 19.3085 | 3.16-44.74 |
| Cotton bollworm | 5 day age | 3.2742X+0.6877 | 20.7517 | 5.78-35.72 |
| Beet armyworm | 1 day age | 4.6966X+2.4965 | 3.4123 | 2.586-4.258 |
| Beet armyworm | 7 day age | 5.1280X+0.8033 | 6.5825 | 4.21-8.956 |
| Diamond-back moth | 2 day age | 3.2638X+0.8616 | 18.5340 | 5.521-25.693 |
| Colcaphellusbowringi | 2 ages | 5.0117X+1.1966 | 5.7399 | 1.4452-10.0346 |
| Cabbage caterpillar | 3 ages | 4.2909X+1.592 | 6.2258 | 3.9805-8.471 |
| Eggplant 18 star ladybugs | 2 ages | 4.8122X+2.4462 | 3.3938 | 1.6308-5.156 |
| Citrus reticulata leaf spiders | Adult | 5.5040X+2.4595 | 2.8969 | 1.9769-3.3168 |
Annotate: the data in the table 4 are the result of the test of tagging.LC
50Unit be μ g/ml.
Studies show that Osthole missible oil all has very strong action of contace poison to having a try worm, but stomach poison function and all low to the toxicity of worm's ovum.
Table 5 0.4% Osthole missible oil part field desinsection drug effect test effect
| The insect title | Crop | Main worm age | Extension rate | Control time | Control efficiency (%) |
| Beet armyworm | The Chinese cabbage seedling | 1-2 age | 800× | After the dispenser 24 hours | 90.0 |
| Cotton bollworm | Cotton | 1-2 age | 800× | After the dispenser 48 hours | 95.1 |
| Cabbage caterpillar | Wild cabbage | 3-4 age | 1000× | After the dispenser 72 hours | 96.9 |
| Tea geometrid | Tealeaves | 2-3 age | 800× | After the dispenser 72 hours | 99.2 |
| Diamond-back moth | Rape | 2-3 age | 800× | After the dispenser 48 hours | 83.2 |
| Two-spotted spider mite | Cotton | Nymph | 1000× | After the dispenser 12 hours | 85.0 |
| Eggplant 18 star ladybugs | Eggplant | 2 ages | 800× | After the dispenser 24 hours | 100 |
Repetition test shows, spray frutus cnidii missible oil after 1-2 hour examination worm with regard to mortality, the continuous and effective phase is no less than 8 days.
The preparation of embodiment 4 0.6% Osthole wettable insecticidal dusts
Produce required instrument and equipment: double worm mixer, injecting type airslide disintegrating mill, vacuum drying chamber, pulvis automatic packaging machine, high pressure liquid chromatograph.
Produce required main medicine and reagent: frutus cnidii insecticide mother liquor (self-control), methyl alcohol, 40% " 961 " pulvis, synergist " 909 ", the withered powder of tea, diatomite, white carbon black, draw back powder.
Production process: Osthole assay in a. frutus cnidii insecticide mother liquor: with embodiment 3.B. weighing: establish preparation 1000kg wetting powder product 1 time, it is as follows to take by weighing various raw materials by table 6:
Table 6 is produced the required various raw materials of 1000kg wetting powder product
| Material name | Requirement (kg) |
| The frutus cnidii insecticide mother liquor | 500 liters |
| The withered powder of tea | 150 |
| " 961 " powder | 60 |
| Synergist " 909 " | 80 |
| Draw back powder | 100 |
| White carbon black | 100 |
| Diatomite | (pact) 480 |
| Semi-finished product weight adds up to | 1000 |
C. Osthole absorption: the diatomite that weighs up, white carbon black, three kinds of raw materials of the withered powder of tea are packed in the double worm mixer into premix 30 minutes.Utilize compressed air the frutus cnidii insecticide mother liquor to be sprayed onto in the premix then, start mixer while spraying and mix by mixer top sprayer unit.D. absorption material oven dry: in vacuum drying chamber, the compound sabot is dried (also can select other drying equipment oven dry for use), 60 ℃～65 ℃ of baking temperatures.E. flour: will draw back powder, " 961 ", " 909 " and the absorption material that makes a good job of through tentatively mixes afterwards with the injecting type airslide disintegrating mill be crushed to about 400 orders Osthole insecticidal dust semi-finished product.F. check: with embodiment 3, but the content X of Osthole in the wetting powder 〉=6000 μ g/g are just qualified.G. the packing: the semi-finished product that are up to the standards are distributed into 50g or 100g pouch-packaged with the pulvis automatic packaging machine, 0.6% Osthole wetting powder product.
The preparation of embodiment 5 0.56% Ah snake's insecticidal emulsifiable concentrates
Produce equipment needed thereby and detecting instrument: preparing tank (stainless steel), automatic filling machine, measuring tank, high pressure liquid chromatograph.
Raw materials for production and reagent: 0.9% (B
1a) abamectin pest killing missible oil, 0.4% Osthole insecticidal emulsifiable concentrate, absolute ethyl alcohol, methyl alcohol.
Production process: establishing an output is 1000 liters.A. feed intake: accurately measure 333 liters of abamectin emulsifiable concentrates by measuring tank earlier, add in the preparing tank, accurately measure the frutus cnidii insecticidal emulsifiable concentrate again by measuring tank then and also add in the above-mentioned preparing tank for 667 liters.B. mixing: start agitator, stirred 30 minutes 0.56% Ah snake's insecticidal emulsifiable concentrate semi-finished product.C. check: with reference to the content X of Osthole in the method detection semi-finished product of embodiment 3, X 〉=0.26% is qualified; With reference to abamectin emulsifiable concentrate company standard (the company standard Q/PY003-1999 of Pingyin subsidiary factory of Qilu Pharmaceutical Factory), press Avermectin B in the HPLC method sampling Detection semi-finished product
1aComponent content Y, Y 〉=0.3% is the qualified (B of the AVM in the product
1bContent does not count).The product that two indexs of X, Y are all qualified just is considered to certified products.D. packing: by automatic filling machine semi-finished product are distributed into 100ml or 250ml bottle, adorn labelled, 0.56% Ah snake's insecticidal emulsifiable concentrate finished product.
Embodiment 6 2.63% snakes kill the wetting powder preparation
Produce equipment needed thereby and detecting instrument: double worm mixer, injecting type airslide disintegrating mill, pulvis automatic packaging machine, high pressure liquid chromatograph.
Produce required main medicine and reagent: 0.6% Osthole wettable powder, general extremely (containing Methomyl 90%SP.), methyl alcohol and Osthole standard items.
Production process (is example once to produce 770 kilograms of products): a. feeds intake: accurately take by weighing Osthole wetting powder 750kg, kill general 20kg, drop in the double worm mixer, mixed 30 minutes.B. pulverize: mixed material is crushed to 400 orders with the injecting type airslide disintegrating mill is 2.63% snake and kills wetting powder semi-finished product (semi-finished product weight is 770 kilograms).C. check: accurately take by weighing snake and kill semi-finished product 1 gram, dilute and nondestructively be transferred to constant volume in the 100ml volumetric flask, be testing sample with the HPLC flowing phase of embodiment 3.Measure the Osthole content X ' that treats in the test sample by embodiment 3 described methods, and measure the content X that snake kills Osthole in the wettable powder.First index of product is qualified when X 〉=0.29%.Go out the content Y of Methomyl in the mixture by the chemical industry standard HG2611-94 of the People's Republic of China (PRC) with high-pressure liquid phase chromatogram therapy determining, second index of product is qualified when Y 〉=2.34%, has only all qualified product of X and Y just can think qualified products.D. packing: above-mentioned semi-finished product are distributed into 50 grams or 100 gram pouches promptly become 2.63% snake and kill the wetting powder product with the pulvis automatic packaging machine.
Claims (7)
1. the purposes of a frutus cnidii ethyl acetate extract is characterized in that the frutus cnidii ethyl acetate extract is used to prepare agricultural chemicals.
2. purposes as claimed in claim 1 is characterized in that wherein said frutus cnidii ethyl acetate extract prepares in order to the below method: after frutus cnidii is pulverized, use the ethyl acetate extracting, concentrating under reduced pressure behind the cracklings removal.
3. purposes as claimed in claim 1, it is characterized in that wherein said frutus cnidii ethyl acetate extract prepares in order to the below method: will be crushed to 40-100 purpose Common Cnidium Fruit and pack in the empty ion exchange column, soak with ethyl acetate, make the extracting that refluxes repeatedly of solvent ethyl acetate, concentrate contain insecticide active substance extract to thick.
4. arbitrary purposes of claim 1 to 3 is characterized in that containing Osthole in the wherein said frutus cnidii ethyl acetate extract.
5. as arbitrary purposes of claim 1 to 3, it is characterized in that the frutus cnidii ethyl acetate extract is mixed with one or more insecticides adjuvants, make agricultural insecticide.
6. as arbitrary purposes of claim 1 to 3, it is characterized in that frutus cnidii ethyl acetate extract and other plant extracts compatibility are made insecticide pesticide.
7. as arbitrary purposes of claim 1 to 3, it is characterized in that frutus cnidii ethyl acetate extract and other agricultural insecticide are mixed, make Recompounded pesticide.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011367881A CN1150826C (en) | 2001-10-25 | 2001-10-25 | Application of cnidium fruit extract in preparing agricultural pesticide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011367881A CN1150826C (en) | 2001-10-25 | 2001-10-25 | Application of cnidium fruit extract in preparing agricultural pesticide |
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| CN1342412A CN1342412A (en) | 2002-04-03 |
| CN1150826C true CN1150826C (en) | 2004-05-26 |
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| CNB011367881A Expired - Fee Related CN1150826C (en) | 2001-10-25 | 2001-10-25 | Application of cnidium fruit extract in preparing agricultural pesticide |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100619146B1 (en) * | 2005-01-04 | 2006-09-01 | 씨제이 주식회사 | Compositions for sterilizing spores of spore-forming microorganisms comprising the extracts of torilidis fructus |
| CN101011051B (en) * | 2006-02-05 | 2010-05-12 | 武汉绿世纪生物工程有限责任公司 | Water dispersion granule for disinsection |
| CN102246825A (en) * | 2011-05-11 | 2011-11-23 | 王乃利 | Biopesticide and preparation method thereof |
| CN103081912B (en) * | 2013-01-25 | 2014-12-10 | 浙江农林大学 | Celastrus angulatus and cnidium lactone compounded pesticide and preparation method thereof |
| CN103601714B (en) * | 2013-08-21 | 2016-12-21 | 陕西康禾立丰生物科技药业有限公司 | Osthole water preparation preparation method and combinations thereof thing |
| CN104396957B (en) * | 2014-10-28 | 2016-08-17 | 青岛青知企业管理咨询有限公司 | For preventing and treating the microemulsion of tea tree tea geometrid |
| CN104692954A (en) * | 2015-03-24 | 2015-06-10 | 江苏大展农业开发有限公司 | Gamma-PGA, fertilizer and pesticide composition preparation method and application in pear garden |
| CN104782689A (en) * | 2015-03-26 | 2015-07-22 | 安徽华宇工艺品集团有限公司 | Pesticide composite for preventing and controlling willow inchworm of yellow husk willow |
| CN104824073A (en) * | 2015-03-26 | 2015-08-12 | 安徽阜南县万家和工艺品有限公司 | A pesticide composition for control of salix sinopurpurea inchworm |
| CN106472616A (en) * | 2016-10-14 | 2017-03-08 | 袁宗英 | A kind of bollworm Pesticidal combination and preparation method thereof |
| CN106879638A (en) * | 2017-02-20 | 2017-06-23 | 李海林 | A kind of new green environment protection insecticide |
| CN109169068A (en) * | 2018-09-28 | 2019-01-11 | 中国科学院动物研究所 | A method of it helps and moves from wheatland to corn field predator |
| CN110506763A (en) * | 2019-09-18 | 2019-11-29 | 浙江省农业科学院 | A kind of novel environment friendly pesticide reagent and preparation method thereof |
| CN115005241B (en) * | 2022-06-30 | 2024-01-26 | 黑龙江省农业科学院齐齐哈尔分院 | Botanical pesticide, preparation method and application thereof |
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