CN1387765A - Germicide containing rhubarb extract and its composition - Google Patents
Germicide containing rhubarb extract and its composition Download PDFInfo
- Publication number
- CN1387765A CN1387765A CN 02123720 CN02123720A CN1387765A CN 1387765 A CN1387765 A CN 1387765A CN 02123720 CN02123720 CN 02123720 CN 02123720 A CN02123720 A CN 02123720A CN 1387765 A CN1387765 A CN 1387765A
- Authority
- CN
- China
- Prior art keywords
- composition
- archen
- chrysophanol
- bactericide
- emodin
- Prior art date
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Links
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- 239000000203 mixture Substances 0.000 title claims abstract description 27
- 241000219061 Rheum Species 0.000 title abstract description 3
- 235000009411 Rheum rhabarbarum Nutrition 0.000 title abstract description 3
- 230000002070 germicidal effect Effects 0.000 title 1
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- 240000001745 Rheum palmatum Species 0.000 claims abstract description 29
- YDQWDHRMZQUTBA-UHFFFAOYSA-N Aloe emodin Chemical compound C1=CC=C2C(=O)C3=CC(CO)=CC(O)=C3C(=O)C2=C1O YDQWDHRMZQUTBA-UHFFFAOYSA-N 0.000 claims abstract description 26
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Abstract
The present invention relates to rhubarb extract and its composition, the plant rhubarb Rheum palmatum is extracted to obtain emodin, chrysophanol, aloe-emodin and their mixture of two or three kinds, then mixed and prepared into agricultural pesticide for crops.
Description
Technical field
The present invention relates to a kind of Chinese rhubarb extract and composition thereof, the invention belongs to pesticide field.
Technical background
Along with development of human society, people are more and more higher to the requirement of environmental protection and food security, and " green agriculture ", " organic farming " have become the direction of agricultural development.And be accompanied by the aggravation of mankind's activity, and environmental deterioration is on the rise, and damage by disease and insect harm is more frequent.The growth of controlling plant pathogen also can be reduced to residue of pesticide minimum effectively, and be that the researcher of pesticide field pursues for people provide non-polluted farm product, utilize Chinese herbal medicine to make the plant sterilization insecticide and become one of effective way for achieving the above object for raw material. alwaysIt is the method that raw material is made plant pesticide with the coptis, cordate houttuynia, peppermint, rheum officinale, Asiatic plantain that Chinese patent application 00129782 discloses a kind of.Chinese patent application 01127595 discloses a kind of method of isolating the total free anthraquinone from Chinese rhubarb compounds from Radix Et Rhizoma Rhei extract, it has the following steps: Radix Et Rhizoma Rhei extract is added acid back heating hydrolysis 1., preferred acid is hydrochloric acid, 2. hydrolyzate is added alkali and regulate pH to 8-10,3. the hydrolyzate after will alkalizing is crossed the anion exchange resin splitter, discard outflow liquid, wash with water to neutrality, 4. with potassium hydroxide one alcoholic solution wash-out, collect eluent, 5. boil off alcohol after in eluent, adding water or not adding water, add acid then and be settled out total free anthraquinone from Chinese rhubarb, be mainly Rhein, archen, aloe-emodin, Chrysophanol, Physcion.But these technology all do not go deep into because of research or operability can't not implemented by force.The present invention is by a large amount of tests, from Chinese herb rhubarb, extract a series of compound, show that through a large amount of tests of pesticide effectiveness it has good preventive and therapeutic effect to a lot of cause of disease of plant, and, have residual low, characteristics such as preventive effect is high, fungicidal spectrum is wide with environmentally compatible.
Summary of the invention
The present invention is that (the Latin name is called: extract archen, Chrysophanol, aloe-emodin and two kinds, three kinds mixtures (hereinafter to be referred as Chinese rhubarb extract) thereof Rheum palmatum) and they are made the various formulations of pesticide and be used for sterilizing from a plant species rheum officinale.
A kind of bactericide that contains Chinese rhubarb extract is characterized in that this bactericide contains Chrysophanol and/or archen and/or aloe-emodin.
Chinese rhubarb extract archen of the present invention, Chrysophanol, aloe-emodin and two kinds, three kinds mixtures thereof can be mixed into composition with other chemical bactericides, and chemical bactericide of the present invention can be any among alkene azoles alcohol, white urea cyanogen, the dimethomorph etc.; Furtherly, composition of the present invention contains alkene azoles alcohol or white urea cyanogen or the dimethomorph of Chinese rhubarb extract such as the archen of 0.01%---90% and/or Chrysophanol and/or aloe-emodin and 0.01%---90%.
Utilize the said composition of the invention described above, be equipped with the known auxiliary agent of those skilled in that art (comprising solvent, filler, synergist etc.) and can make multiple formulation of the present invention, its active constituent content is:
Chinese rhubarb extract archen and/or Chrysophanol and/or aloe-emodin 0.01%---90%
Alkene azoles alcohol or white urea cyanogen or dimethomorph 0.01%---90%
The formulation that the present invention may process is:
A, missible oil
B, wetting powder
C, oil-suspending agent
D, aqueous suspension agent
A, missible oil are can be one or more compositions among methyl alcohol, ethanol, chloroform, dimethylbenzene, the toluene etc. by active ingredient being dissolved in one or more organic solvents, being used for solvent of the present invention; Be used for emulsifier of the present invention and can be one or more materials among poly alkyl alcohol ethylene glycol sulphate, fatty acid amide N-methyl Taurine sodium salt, the sodium sulfate of polyethenoxy ether of fatty alcohol, consumption is 1---30% usually; The present invention also comprises penetrant t, azone, YZ-901, and consumption is 0.1---20% usually.
B, wetting powder are can homodisperse preparation in water, wetting powder of the present invention is except that being added with thinners such as white carbon black, precipitated calcium carbonate, potter's clay, diatomite or inert substance, it contains ionic or nonionic surface active agent (wetting agent, dispersant), for example: fatty alcohol polyglycol ether sulphate, fatty acid amide N-methyl Taurine sodium salt, sodium sulfate of polyethenoxy ether of fatty alcohol, neopelex-calcium, sodium lignin sulfonate-calcium, one or more materials among the SOPA etc., content are 1-30%; It is 0.1---20% that the present invention also comprises penetrant t, azone, the common consumption of YZ-901.
C, oil-suspending agent are to be made by former medicine, surfactant adding mineral oil or vegetable oil, surfactant of the present invention comprises the liquid ester class of phthalic acid dimethyl ester, fourth fat, two isobutyl fat, two laruyl alcohol esters, two cyclic esters, two cyclohexanols, two ring monooctyl esters and fatty acid, fatty alcohol, consumption 1-80% usually; Can be fatty alcohol polyglycol ether sulphate, fatty acid amide N methyl taurine sodium salt, sodium sulfate of polyethenoxy ether of fatty alcohol, neopelex-calcium, sodium lignin sulfonate-calcium, the SOPA of emulsifier, usually consumption 1-30%.
D; aqueous suspension agent is that the extract of rheum officinale and alkene azoles alcohol or white urea cyanogen or dimethomorph are used with; adding synergist; behind the auxiliary agent; through ball milling; the preparation that sand milling is made; auxiliary agent of the present invention can be a fatty alcohol polyglycol ether sulphate; fatty acid amide N methyl taurine sodium salt; sodium sulfate of polyethenoxy ether of fatty alcohol; neopelex-calcium; sodium lignin sulfonate-calcium; alkylphenol polyoxyethylene; one or more materials among the triphen ethyl-phenol polyoxyethylene; common consumption 1---30%; the present invention also contains penetrant t; common consumption 0.1---30%, ethylene glycol; CMC; the common consumption 0.1---10% of xanthans.
The optimum ratio of microbicide compositions of the present invention is (percentage by weight):
Archen and/or Chrysophanol and/or aloe-emodin 0.1---60%
Alkene azoles alcohol or white urea cyanogen or dimethomorph 0.1---90%
Auxiliary agent is OP---10,0201,0203, farming breast 500,1600,1601,1602,2201,0208, detergent alkylate yellow acid Sodium, any one among lignin yellow acid Sodium, the SOPA or multiple composition, consumption 1---30% usually.
Synergist is any one or the multiple composition among penetrant t, azone, the YZ---901, usually consumption 1---30%.
Filler be in CMC, xanthans, white carbon black, potter's clay, the diatomite any one or multiple composition, consumption 0.1---80% usually.
Take by weighing each component according to said ratio, can be made into wetting powder of the present invention through formulated.
The optimum formula of archen bactericide of the present invention is:
Archen 0.2%
SOPA 15％
Ethanol 20%
Dimethylbenzene complements to 100%
The more existing technology of bactericide of the present invention has been compared following advantage:
1, noresidue.Product of the present invention is a public nuisance-free agricultural chemicals.
2, fungicidal spectrum extensively has good preventive and therapeutic effect to multiple bacterium.
3, synergistic effect is obvious.
Brief Description Of Drawings:
Fig. 1 extracts flow chart for rheum officinale main component of the present invention
Fig. 2 is the preventive effect change curve of Chinese rhubarb extract of the present invention to powdery mildew of cucumber
Embodiment: Chinese rhubarb extract of the present invention is prevented and treated research report 1 material of powdery mildew of cucumber and method 1.1 material 1.1.1 vegetable material rheum officinales, and (the Latin name is called: 1.1.2 bacterial classification powdery mildew of cucumber bacterium (Sphaerotheca fuliginea) (picking up from the Institute of Plant Protection, Hebei province) Rheum palmatum); Botrytis cinerea (Botrytis cinerea), root rotof flax bacterium 20 kinds of pathogenic bacteria (Hebei agricultural university toxin chamber provides) 1.1.3 cucumber variety Chang Chun Mi Cis such as (Cochliobolus sativus) (Great Wall, Chengde kind industry company) 1.1.4 chemical agent 15% triadimefon WP (Zhangjagang City second insecticide factory); 20% nitrile bacterium azoles WP (Zhejiang one sail insecticide factory) 1.1.5 medicine and instrument
The preparation of the primary dcreening operation 1.2.1.1 rheum officinale crude extract of absolute ethyl alcohol, ether, sodium carbonate, sodium bicarbonate, hydrochloric acid, chloroform, pyridine, isoamyl alcohol (it is pure to be analysis) Fs-100 micromill, rotary evaporator, centrifuge 1.2 method 1.2.1 rheum officinale crude extracts
Rheum officinale pulverizing → extraction (Chinese herbal medicine: 80% ethanol=1: 5 (w/v)) → vibration (2d, 150rmin
-1, 25 ℃) → centrifugal (3500rmin
-1, 20min) get supernatant → 40 ℃ rotary evaporation → with 80% ethanol constant volume (soup milliliter number and rheum officinale gram number equates) → 4 ℃ of refrigerators preservations are standby.1.2.1.2 the cultivation of cucumber seedling
Adopt soilless culture method, the plastics greenhouse by solar heat spring stubble that reference literature is introduced is the cucumber cultivation technology early.1.2.1.3 the preservation of powdery mildew bacterial classification
To be used to preserve the cucumber seedling cucumber seedling isolation used with test of bacterial classification, inoculation is cultivated standby in 20 ℃～24 ℃ greenhouse.1.2.1.4 inoculation
Adopt the back 9 days incidence of leaf of inoculation, conidium is brushed in the beaker that fills clear water, it is made into about 20 the conidial suspension in every visual field under 10 * 10 power microscopes with writing brush.Spore suspension is sprayed on brokenly uniformly on the blade of heart stage plant then.1.2.1.5 protection and result of treatment are measured
At the broken heart stage spray of cucumber extract; if clear water, 80% ethanol and chemical agent (protection measure of merit 1000 times of liquid of triadimefon; result of treatment test 3000 times of liquid of nitrile bacterium azoles) contrast; each handles 10 strains; place under 24 ℃～26 ℃, Polypropylence Sheet covers and preserves moisture, and treats to investigate when the clear water contrast is fully fallen ill and respectively handles the state of an illness; the record severity calculates disease index and preventive effect.Protection and result of treatment be the preceding 24h of finger kind and the effect of inoculating back 24h spray medicine (protective effect is tested with 50 times of liquid, and therapeutic action is tested with 100 times of liquid) respectively.
Rate * 100 of disease index (%)=average severity * generally
Preventive effect (%)=(the contrast disease refers to-handle that disease refers to)/contrast disease index * 1001.2.2 toxicity test
Crude extract is diluted 600,800,1000,1200,1400,1600,1800 times respectively, test its protective effect then, calculate Ec50 and Ec90 powdery mildew of cucumber.1.2.3 lasting period test
Before inoculation 1,2,3,4,5,6d handles 10 strain seedling with 100 times of liquid of crude extract, and 1d establishes the then unified inoculation of clear water, 80% ethanol, 1000 times of control treatment such as liquid of triadimefon before inoculation, treat to investigate when the clear water contrast is seriously fallen ill and respectively handle severity and write down the result, calculate disease index and preventive effect.1.2.4 the test of antimicrobial spectrum
The 1mL extract is joined in the PDA medium that 100mL melts, fall ware (d=9cm), play bacterium dish inoculation (establish clear water, 80% ethanol compares, 4 repetitions of every processing) with the card punch of d=0.6cm.Put into 25 ℃ of constant incubators and cultivate, wait to contrast bacterium colony length and to about 7cm, measure colony diameter, and calculate inhibiting rate.
Inhibiting rate (%)=(the clean amount of growth of CK-handle clean the amount of growth)/clean amount of growth of CK * 100
Annotate: main component active testing in clean amount of growth=colony diameter-bacterium dish diameter 1.2.5 rheum officinale
Standard items Rhein, Chrysophanol are diluted 500x, 1000x with pyridine, anhydrous alcohol solution respectively, add water then and continue 10,000,50,000,100,000,200,000 times of 4 concentration of dilution, archen is established clear water, 10%, 2%, 1%, 0.5% pyridine and 10%, 2%, 1%, its activity of 0.5% ethanol contrast survey then with 10% ethanol dilution 500x and 1000x.Use archen, Rhein, Chrysophanol and the Physcion etc. that are extracted slightly to put forward the protection activity of 1000 times of liquid tests of product simultaneously to the powdery mildew of cucumber bacterium.1.2.7 with the chemical agent proportioning test
Crude extract is made 0.2% aqua, with alkene azoles alcohol by active ingredient than 3: 1,1: 1,3 ratios such as 1: 3 grade were mixed, and surveyed the Ec50 of itself and each single agent then respectively, calculated its co-toxicity coefficient.2 results and the test result and analysis 2.1.1 protective effect test result of analysis 2.1 rheum officinale crude extracts to the protection and the therapeutic action of powdery mildew of cucumber
Rheum officinale plant crude extract activity is higher, and its 50 times of liquid preventive effects and 1000 times of liquid of chemical agent triadimefon are in same significance level.
Table 1 Chinese rhubarb extract is to the protection measure of merit result of powdery mildew of cucumber
Handle generally rate/% disease index/% preventive effect/% significance of difference of average severity/%
Triadimefon 2.00 40.00 0.80 98.90 ns
Rheum officinale 23.25 100.00 23.25 73.04 ns
80% ethanol, 86.00 100.00 86.00 0.29 * *
Clear water 86.25 100.00 86.25 0.00 * *
Triadimefon 4.00 40.00 1.60 98.07 ns
Rheum officinale 30.00 100.00 24.00 71.08 ns
Clear water 83.00 100.00 83.00 0.00 * *
80% ethanol, 88.00 100.00 88.00-6.02 * *
Annotate: ns represents that difference is not remarkable between processing and the triadimefon;
*Significant difference between expression processing and the triadimefon
(confidence level is 0.05);
*Expression handle and triadimefon between difference extremely significantly (confidence level is 0.01).
Be the different batches separator bar.2.2 rheum officinale virulence test result and analysis
According to Fig. 2 Chinese rhubarb extract the preventive effect change trend curve of powdery mildew of cucumber is obtained its relevant fit equation: y=-1.7706x
2-2.6837x+107.51 (R
2=0.9882), calculating Chinese rhubarb extract according to this equation is 1398.30 times to the Ec50 of powdery mildew of cucumber, and its Ec90 is 1051.21 times.2.3 the lasting period test result of the protective effect of rheum officinale
As can be seen from Table 2,1d～6d sprays 100 times of liquid of Chinese rhubarb extract in advance, and its preventive effect significantly is better than 1000 times of liquid of triadimefon all more than 90%, can draw thus, and the lasting period of the protective effect of Chinese rhubarb extract can reach 6d at least.
Table 2 Chinese rhubarb extract is to the lasting period of powdery mildew of cucumber bacterium protective effect
Handle extremely significantly water of disease index preventive effect/% 5% remarkable water 1%
/ % is average
80% ethanol, 89.13-2.31 a A
Clear water 87.12 0.00 a A
Triadimefon 22.16 73.41 b B
1d 8.59 92.60 c C before the inoculation
6d 6.42 92.60 c C before the inoculation
5d 4.17 95.63 c C before the inoculation
2d 2.11 97.57 c C before the inoculation
4d 1.52 98.27 c C before the inoculation
The test result of 3d 0.30 99.65 c C2.4 Chinese rhubarb extract antimicrobial spectrum before the inoculation
As can be seen from Table 3,100 times of liquid of Chinese rhubarb extract all have certain inhibitory action to 20 kinds of fungies for examination, wherein inhibiting rate reaches have 10 kinds more than 50%, account for for 50% of examination bacterium, and root rotof flax bacterium (Cochliobolus sativus) and Exserohilum turcicum (Exserohilum turcicum) inhibiting rate have been reached about 80%.
Table 3 Chinese rhubarb extract is to the inhibitory action of 20 kinds of pathomycete colony diameters
80% ethanol TS-109,80% ethanol TS-109
Supply the examination fungi for the examination fungi
Bacteriostasis rate/% bacteriostasis rate/% bacteriostasis rate/% bacteriostasis rate/%
Cochliobolus?sativus 2.58 82.21 Alternaria?solani 9.09 49.79
Exserohilum?turcicum -33.40 79.69 Colletotrichum?graminicola 5.84 49.04
Gibberella?zeae 9.36 66.00 Alternaria?porri 5.21 47.13
Rhizoctonia?solani 25.79 63.06 Fusarium?graminearum -20.29 43.97
Pythium?gramineacola 3.42 60.57 Rizoctonia?cerealis -4.87 42.11
Fusarium?moniliforme 8.06 60.28 Leptosphaeria?maydis -4.84 41.09
Botryosphaeria?berengeriana?-6.46 58.14 Colletotrichum?gossypii 4.70 33.37
Curvularia?lunata 5.82 56.66 Alternaria?kikuchiana 1.34 30.54
Colletotrichum?capsici 3.09 51.97 Alternaria?mali -1.15 21.47
Fusarium oxysporum 16.46 51.92 Verticillium dahliae-3.37 20.452.5 Chinese rhubarb extract active ingredient qualification results
As can be seen from Table 4, the standard items Rhein is to the cucumber powdery mildew fungus non-activity, and archen shows certain activity, and Chrysophanol shows high activity, and the preventive effect of its 10000 times of liquid and 3000 times of liquid of alkene azoles alcohol is in same significance level.As can be seen from Table 5, slightly carry the product Rhein to powdery mildew of cucumber bacterium non-activity, and archen, Chrysophanol and Physcion show greater activity.Therefore can draw: Rhein is a non-active ingredients of preventing and treating powdery mildew, and archen and Chrysophanol are its active ingredient.
The active testing result (standard items) of main component in table 4 rheum officinale
Handle disease index/% preventive effect/% 5% significance level 1% utmost point significance level
10% ethanol, 97.8105-7.78 a A
2.0% ethanol, 94.7497-4.44 a A
Rhein
(50,000 times)94.1514-3.70 a A
Rhein
(100,000 times)94.1439-3.70 a A
2.0% pyridine, 92.7700-2.22 a A
Rhein
(200,000 times)91.7715-1.23 a A
0.5% pyridine, 91.7565-1.11 a A
1.0% pyridine, 90.7835 0.00 a A
Clear water 90.7565 0.00 a A
Rhein
(10,000 times)88.5658 2.47 a A
1.0% ethanol, 84.6417 6.67 a A
0.5% ethanol, 83.1687 8.33 a A
Chrysophanol
(200,000 times)52.4120 42.22 b B
Chrysophanol
(100,000 times)51.4458 43.33 b B
Chrysophanol
(50,000 times)34.0404 62.56 c B
Archen
(1000 times)0.5000 94.49 d C
Archen
(500 times)0.3000 96.69 d C
Chrysophanol
(10,000 times)0.0000 100.00 d C
Alkene azoles alcohol
(3000x)0.0000 100.00 d C
Main component determination of activity result (slightly carrying product) in table 5 Radix Et Rhizoma Rhei extract
Handle disease index/% preventive effect/% 5% significance level 1% utmost point significance level
80% ethanol, 100.00-8.70 a A
Clear water 92.00 0.00 a A
Rhein 90.00 2.17 a A
Archen 10.80 88.26 b B
Chrysophanol and 0.800 99.13 b B
The proportioning test result of Physcion 2.5 Chinese rhubarb extracts and alkene azoles alcohol:
Draw by the virulence equation: alkene azoles alcohol Ec50=0.523ppm
Chinese rhubarb extract Ec50=0.970ppm Chinese rhubarb extract: alkene azoles alcohol Ec50ppm co-toxicity coefficient
3∶1 0.986 121.06
1∶1 0.282 240.98
1: 3 0.603 138.02 by co-toxicity coefficient as can be known, and the active ingredient of Chinese rhubarb extract and alkene azoles alcohol is in 3: 1-1: 3 ratio proportioning has obvious synergistic effect, and the two can be mixed in this ratio.
The technology of knowing altogether with personnel in this area, can draw Chrysophanol and/or archen and/or aloe-emodin pure or white urea cyanogen or the composite co-toxicity coefficient of dimethomorph with the alkene azoles respectively as stated above respectively, promptly at Chrysophanol and/or archen and/or aloe-emodin 0.01%---90%, composite in the scope of alkene azoles alcohol or white urea cyanogen or dimethomorph 0.1%---90% have an obvious synergistic effect.
Two, formulation Example:
According to the number range of each material of the present invention, the amount that takes by weighing active ingredient, auxiliary agent, emulsifier, solvent can be prepared missible oil of the present invention, and same method can make wetting powder of the present invention, oil-suspending agent, aqueous suspension agent etc.
Claims (5)
1, the bactericide that contains Chinese rhubarb extract is characterized in that this bactericide contains Chrysophanol and/or archen and/or aloe-emodin.
2, bactericide according to claim 1 is characterized in that it can become composition with alkene azoles alcohol or white urea cyanogen or dimethomorph proportioning.
3, bactericide according to claim 1 is characterized in that the optimum formula of archen bactericide is:
Archen 0.2%
SOPA 15％
Ethanol 20%
Dimethylbenzene complements to 100%
4, composition according to claim 2 is characterized in that said composition contains:
Chrysophanol and/or archen and/or aloe-emodin 0.01%---90%
Alkene azoles alcohol or white urea cyanogen or dimethomorph 0.1%---90%.
5, composition according to claim 2 is characterized in that the preferred percentage by weight of said composition consists of:
Archen and/or Chrysophanol and/or aloe-emodin 0.1---60%
Alkene azoles alcohol or white urea cyanogen or dimethomorph 0.1---90%
Auxiliary agent is OP---10,0201,0203, farming breast 500,1600,1601,1602,2201,0208, detergent alkylate yellow acid Sodium, any one among lignin yellow acid Sodium, the SOPA or multiple composition, consumption 1---30%
Synergist is any one or the multiple composition among penetrant t, azone, the YZ---901, consumption 1---30%
Filler be in CMC, xanthans, white carbon black, potter's clay, the diatomite any one or multiple composition, consumption 0.1---80%.
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Effective date of registration: 20190404 Address after: 712100 North Side of Qingxin Road, Small and Medium-sized Enterprise Park, Wuquan Town, Yangling Demonstration Area, Xianyang City, Shaanxi Province Patentee after: YANGLING FJ BIOTECHNOLOGY CO.,LTD. Address before: 518123 3rd floor, 21 Jinnan Road, Nanwan Street, Longgang District, Shenzhen City, Guangdong Province Patentee before: SHENZHEN QIANHAI FJ BIOLOGICAL TECHNOLOGY DEVELOPMENT Co.,Ltd. |
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