CN1229584A - Insecticide containing organic nitrogen and organic phosphorus compound, its prepn. method and application - Google Patents

Insecticide containing organic nitrogen and organic phosphorus compound, its prepn. method and application Download PDF

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Publication number
CN1229584A
CN1229584A CN 98101116 CN98101116A CN1229584A CN 1229584 A CN1229584 A CN 1229584A CN 98101116 CN98101116 CN 98101116 CN 98101116 A CN98101116 A CN 98101116A CN 1229584 A CN1229584 A CN 1229584A
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Prior art keywords
carbofuran
granule
chlorophos
sand
insecticide
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全文忠
刘明森
熊建峰
邢春奎
金新瑞
周朝品
全建敏
全晓静
刘敏
张志峰
周延平
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YUXIPENGCHENG CHEMICAL AND METALLURGICAL CORP CHEMICAL PLANT
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YUXIPENGCHENG CHEMICAL AND METALLURGICAL CORP CHEMICAL PLANT
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Abstract

An insecticide in the form of particles for preventing and eliminating cotton aphis, corn borer, peanut threadworm and cane cutworm is prepared from sand as carrier, polyvinyl alcohol as adhesive to be coated on the surface of sand, and Kebaiwei and trichlorfon (0.2-2.8%) coated around the sand, and features lower poison broad spectrum and delayed resistance of pests.

Description

Contain insecticide of organic nitrogen and organic phosphorus compound and its production and use
The present invention relates to contain insecticide, preparation method and the purposes of organic nitrogen and organic phosphorus compound, specifically, the present invention relates to the composite granule of carbofuran and chlorophos, can be used as the insecticide of cotten aphid, corn borer, peanut nematode and sugarcane field tiger.
The 3% carbofuran granule cotton plant rhizosphere of spreading manuer in holes has preventive effect preferably to cotten aphid, but on the high side, toxicity is also bigger than normal.Therefore be necessary to develop and overcome these shortcomings but do not subtract the new carbofuran preparation of its drug effect, to replace 3% carbofuran particle.
Known carbofuran, chemical name are 2,3-dihydro-2,2-dimethyl-7-benzofuranyl-methyl carbamate.Its biologically active is a kind of broad spectrum insecticide, kill mite, nematocide.Have very strong interior absorption, insect is had tag, stomach poison function.Former medicine big white mouse acute oral LD 50Be 8-14mg/kg, to the high poison of people, animal.Can be used for the control of various pests such as cotton, paddy rice, sugarcane, tea, peanut.
Chlorophos, chemical name O, O-dimethyl-(2,2,2-three chloro-1-ethoxys) phosphonate ester.Insect there are stronger stomach poison function and action of contace poison, and have permeability.Former medicine big white mouse acute oral LD 50560-630mg/kg is to the people, animal low toxicity.Can be used for preventing and treating paddy rice, tea, really, the insect pest of crop such as vegetables.
Have now found that the composite granule of carbofuran and chlorophos has the preventive effect identical with the carbofuran granule under same consumption, but toxicity reduces significantly, but and suspension of pesticide resistance generation.
Thus, the object of the present invention is to provide a kind of is carbofuran-chlorophos granular insecticide of 3% by granule weight total amount, and commodity are called 3% Kediwei, this granule high-efficiency low-toxicity.
Second purpose of the present invention is to provide the method for producing above-mentioned 3% carbofuran-chlorophos granular insecticide.
The 3rd purpose of the present invention is the application of above-mentioned 3% carbofuran-chlorophos granule as cotten aphid, corn borer, peanut nematode and sugarcane field tiger insecticide.
In order to finish task of the present invention, adopt following technical scheme.
A kind of granular insecticide, this granular insecticide are that carrier outsourcing total amount is the carbofuran and the chlorophos of 3% (by granule weight) in sand.
In the granule of the present invention the content of active ingredient carbofuran by granule weight in the scope of 0.2-2.8%, preferred 0.5-2.5%, more preferably 1.0-2.0%.
The carbofuran that is used for the present invention, granularity are more than 200 orders, and available from the Hunan Chemical Research Institute test site, trade mark is extra large sharp board.
The used chlorophos of the present invention is 90% chlorophos pulvis of our factory's production.Production method is the known technology that record is gone up by " chemical industry complete works " (the refined chief editor of plum, Chemical Industry Press).
As carrier, the preferred river of the present invention sand, other is the sand of main component with calcium carbonate, also can use.The preferred 16-50 order of the granularity of sand, % (mass ratio) 〉=95.
In order to be processed into granular pesticide by former medicine, carrier and adjuvant, when making particle, also used polyvinyl alcohol and colouring agent alkalescence crystal violet as binding agent, be insecticide as the aubergine warning colouration to distinguish and to identify granule of the present invention.The polyvinyl alcohol consumption is 0.17% of a granule weight, and alkaline crystal violet is 0.1%.
The production method of above-mentioned 3% carbofuran-chlorophos granule comprises following step successively:
(1) screening and oven dry sand;
(2) with polyvinyl alcohol: alkaline crystal violet: water=1.7: 1: the 15-17 weight ratio is mixed each material, and to neutral, heating gets painted binding agent liquid, this liquid is added in the resulting sand of step (1) and with it mix with the sour solution of transferring;
(3) add the carbofuran of 0.2%-2.8% in step (2) the gained mixture by granule weight, mixing;
(4) with chlorophos: methyl alcohol=weight ratio made the chlorophos methanol solution in 3: 1, this solution was added in step (3) the gained mixture mixing;
(5) oven dry.
Being used for the present invention's sand fineness, so select the 16-50 order, is because the carrier grains of sand are spent greatly, easily come off when sand collides as the carbofuran and the chlorophos of dressing, and during undersized, carbofuran and chlorophos is difficult for wrapping on the surface of carrier sand.Through evidence 16 orders-50 order, the sand of 〉=95% (quality) is optimal.
Water content≤0.5% of sand before the preferred dressing.This is because if the sand grains water content in the finished product when too high, in order to slough redundant moisture, is had under higher temperature or the time expand oven dry, does not only uneconomically like this, but also can cause the thermolysis of carbofuran and chlorophos.
For the water that guarantees that the active ingredient in 3% carbofuran-chlorophos granule does not reduce, must manage to remove in the technical process as much as possible to be added.Consider that carbofuran is higher than 175 ℃ in temperature and begins at once to decompose, chlorophos begins to decompose at 115 ℃, so the inventor is chosen in 65-90 ℃ of hot-air, stirs 30 rev/mins of revolutions, and drying time is under 30-50 minute the condition, to carry out baking test.Result of the test shows, the oven dry optimum condition: with 70-80 ℃ hot-air; Stirring the commentaries on classics effect is 30 rev/mins; Time is 30-45 minute.
Granular insecticide of the present invention forms owing to be that carbofuran and chlorophos are composite, so enlarged insecticidal spectrum, under the situation that preventive effect does not reduce, has significantly reduced toxicity.Again because the price of chlorophos is much lower far beyond carbofuran, so composite granule price is much lower far beyond single carbofuran granule.
Below with reference to embodiment the present invention is done more specifically, illustrates without limitation, and advantage of the present invention is done announcement more fully.Embodiment 1-produces 3% carbofuran-chlorophos granule.
Get the 16-50 order that sieves, 〉=95% (by quality) and moisture content are lower than 0.5% river sand 967.3kg, put into mixer.
In another container that can heat, add 15kg water, add 1kg alkalescence crystal violet and 1.7kg polyvinyl alcohol then successively, be heated to 50-60 ℃, get the binding agent liquid of a uniform coloring, under agitation add mixer.Add the carbofuran of 20kg then greater than 200 order fine powders, after fully stirring, add 10kg chlorophos again in the mixer and be dissolved in solution in the 3.4kg methyl alcohol, stop the agitator running after fully stirring, material in the mixture is transferred to removes moisture in the warm air drier, treating that moisture reaches is lower than at 0.8% o'clock, sends to packing, obtains finished product.Finished product expulsion rate≤5% (quality).Embodiment 2-field control effectiveness test.
The agriculture chemical examination institution, Shandong Province carried out field control effectiveness test for agriculture chemical registration and large scale application provide scientific basis to 3% carbofuran-chlorophos granule control cotten aphid in 1996.
1, reagent agent:
3% carbofuran-chlorophos granule (Yuxipengcheng Chemical and Metallurgical Corp., Chemical Plant's production);
3% carbofuran granule (production of Shandong insecticide factory of Ningyang).
2, controlling object: cotten aphid.
3, experimental scheme and processing:
Handle 1 3% carbofuran-chlorophos granule 1.5kg/ mu;
Handle 2 3% carbofurans-chlorophos granule 2.0kg/ mu;
Handle 3 3% carbofurans-chlorophos granule 2.5kg/ mu;
Handle 4 3% carbofuran granule 2.0kg/ mus;
Handle 5 blanks.
This test is totally 5 processing, repeats totally two ten sub-districts, 40 square metres of sub-district areas, randomized arrangement four times.
4, test basic condition:
No. 12, cotton variety middle cotton of test, growing way is medium, and cotten aphid is taken place heavier.The individual plant formulation rate is respectively handled in conversion, and individual plant only imposes on the cotton plant rhizosphere.
5, investigation and calculating:
Every sub-district is by 5 samplings of diagonal method, every two strain, last two fruit branches of every strain investigation, every sub-district is investigated 20 fruit branches altogether, investigation insect population radix was investigated residual borer population in 7,20 days behind the medicine, calculate insect population go down rate with proofread and correct preventive effect.
6, result of the test:
(1) result of the test sees Table 1;
(2) 3% carbofurans-chlorophos granule mu consumption 1.5kg, 2kg, 2.5kg, preventive effect was respectively 93%, 93.4% and 94.5% in 7 days, preventive effect was respectively 92.5%, 94.2% and 957% in 20 days, contrast medicament 3% carbofuran granule mu consumption 2.0kg, preventive effect was respectively 93.3%, 95.0% in 7 days, 20 days;
The anti-no significant difference that produces of (3) 3% carbofurans-three dosage of chlorophos granule is considered to be advisable with 2.0kg/ mu from economical and effective;
(4) no poisoning phenomenon is handled in test.Embodiment 3-field control effectiveness test
The agriculture chemical examination institution, Henan Province applied for agriculture chemical registration and enlarged-area in 1997 foundation is provided, and estimated the control efficiency of 3% carbofuran-chlorophos granule to cotten aphid, determined that optimal dose tests.
1, reagent agent:
3% carbofuran-chlorophos granule (Yuxipengcheng Chemical and Metallurgical Corp., Chemical Plant provides);
Contrast medicament 3% carbofuran granule (Jiangsu brass hill insecticide factory).
2, controlling object: cotten aphid.
3, test kind: in 375, summer flower, dibbling behind the wheat, growing way is medium, it is heavier that cotten aphid is taken place, several 4000 strains of mu strain.
4, experimental scheme:
(1) 5 processing are established in test, repeat totally 20 sub-districts, every sub-district area 30m for 4 times 2, the sub-district randomized arrangement respectively is treated to:
A, 3% carbofuran-chlorophos granule 1.5kg/ mu;
B, 3% carbofuran-chlorophos granule 2.0kg/ mu;
C, 3% carbofuran-chlorophos granule 2.5kg/ mu;
D, 3% carbofuran Granules 2.0kg/ mu;
E, blank.
(2) test when cotten aphid is sporadicly taken place, by the sub-district area, the individual plant formulation rate is respectively handled in conversion before the dispenser, and individual plant is spreaded manuer in holes in the cotton plant rhizosphere.
(3) investigation method is identical with embodiment 2: radix before the record dispenser, and 7 days, 15 days and 30 days cotten aphid quantity after the dispenser, and calculate go down rate and proofread and correct preventive effect of 7,15 and 30 days insect populations according to relevant formula.
5, interpretation of result:
After (1) 3% carbofuran-chlorophos granule dispenser 7,15,30 days insect populations go down rate, proofread and correct preventive effect and see Table 2.
As shown in Table 2: 3% carbofuran-chlorophos granule control cotten aphid, with mu 2.5kg best results, 7,15,30 days correction preventive effects are 97.7%, 95.3%, 88.8% behind the medicine.Mu is used 2kg, and 7,15 days correction preventive effects are suitable with contrast medicine 2kg/ mu behind the medicine, are lower than the contrast medicine but held in 30 days to imitate.7,15,30 days correction preventive effects are respectively behind both medicines: 93.4%, 94.6%, 79.5%, 93.5%, 94.2%, 85.8%.The poorest with 3% carbofuran-chlorophos granule 1.5kg/ mu effect, 7,15,30 days correction preventive effects are 85.8%, 90.3%, 54.1% behind its medicine.
(2) proofread and correct preventive effect in 15 days after utilizing DMR T method to medicine and carry out variance analysis, the results are shown in Table 3.
As shown in Table 3: 3% carbofuran-chlorophos granule mu does not have significant difference with 2kg, 2.5kg and contrast medicine 2kg preventive effect, but the three all extremely significantly is better than 3% carbofuran-chlorophos granule 1.5kg/ mu, so control cotten aphid optimal dose is 3% carbofuran-chlorophos granule 2kg/ mu.
Poisoning and other bad phenomenon are not found in test.Embodiment 4-agricultural chemicals acute toxicity testing
1997, preclinical medicine institute of Henan Medical Univ. pharmacology is teaching and research to be studied carefully once 3% carbofuran-chlorophos granule was carried out acute toxicity experience.
Agricultural chemicals 3% carbofuran-chlorophos granule is provided by Yuxipengcheng Chemical and Metallurgical Corp., Chemical Plant, is diluted to desired concn with distilled water is low than method during experiment.
60 of animal Wistar big white mouse, body weight 180-220g, random packet.Henan Medical Univ.'s Experimental Animal Center provides.
Method (1) acute oral contamination: according to the trial test result, establish 245,307,384, four dosage groups of 480mg/kg, between group than 0.8,10 of every group of rats, male and female half and half.The animal fasting is 12 hours before the administration, freely drinks water, and each group difference is gastric infusion once, and the 1ml/kg body weight is contaminated and recovered in back 2 hours to observe the reaction of animals situation, continuous 2 weeks for food.
(2) acute through skin: as, to establish dosage group of 2000mg/kg according to the trial test result.20 of rats, male and female half and half, preceding 24 hours of coating shaves off the back part of animal hair, area 4 * 5cm 2, soup is applied to the unhairing district, with about 20cm 2The cover box be fixed in the unhairing district.Take off the cover box after making soup and skin continue to contact 4 hours,, continue to observe toxic reaction, continuous 2 weeks with the remaining agricultural chemicals of warm water flush away.
Result: (1) acute oral: contaminate after 5-10 minute, animal occurs delay of response, hydrostomia in succession, trembles, symptoms such as respiratory secretions increases, eyeball congestion, act tail, animal dead was all arranged in 24 hours, the postmortem dead animal, each internal organs of perusal show no obvious abnormalities.Not dead animal is many to reactivate and took food after 24 hours, observed for 2 weeks continuously, and the weight of animals recovers gradually and increases, and movable feed is normal.Dosage group lethality (P) is respectively from high to low: 0.90,0.70,0.40,0.10, and according to each treated animal death toll, this median effective dose probit method-weighted regression method statistical disposition, the result:
LD 50=335.86mg/kg;
LD 5095% credibility interval: 297.11-374.1mg/kg.
(2) acute through skin: contaminating occurred slightly trembling after 3 hours, and after 24 hours, it is normal that movable feed recovers gradually, observed for 2 weeks continuously, and body weight is not seen obviously and alleviated, and increases by 20 none death of animal, the LD of this medicine gradually 50Greater than 2000mg/kg.
Conclusion: according to the existing agricultural chemicals acute toxicity grading criteria of China, for trying agricultural chemicals the contamination of rat acute per os is poisoning, acute is low-toxin farm chemicals through the skin contamination.
Table 1 3% carbofuran chlorophos granule control cotten aphid effect research table
Test is handled Repeat Insect population radix before the medicine After the dispenser 7 days After the dispenser 20 days
Residual borer population The insect population rate (%) that goes down Proofread and correct preventive effect (%) Residual borer population The insect population rate (%) that goes down Proofread and correct preventive effect (%)
3% carbofuran chlorophos granule 1.5kg/ mu ??1 ????38 ????23 ????39.5 ????91.3 ????189 ??-397.4 ????92.0
??2 ????36 ????16 ????55.6 ????94.3 ????250 ??-594.4 ????93.3
??3 ????26 ????15 ????42.3 ????90.4 ????285 ??-996.2 ????88.9
??4 ????30 ????11 ????63.3 ????95.9 ????187 ??-523.3 ????95.8
??X ????93.0 ????92.5
3% carbofuran chlorophos granule 2.0kg/ mu ??1 ????35 ????16 ????54.3 ????93.5 ????136 ??-288.6 ????93.8
??2 ????39 ????18 ????53.8 ????94.0 ????120 ??-2077 ????97.0
??3 ????27 ????14 ????48.1 ????91.4 ????200 ??-640.7 ????88.2
??4 ????40 ????19 ????52.5 ????94.6 ????135 ??-237.5 ????94.2
??X
3% carbofuran chlorophos granule 2.5kg/ mu ??1 ????34 ????13 ????61.8 ????94.5 ????95 ??-179.4 ????95.5
??2 ????37 ????15 ????59.5 ????94.8 ????121 ??-227.0 ????96.8
??3 ????28 ????12 ????57.1 ????92.9 ????118 ??-321?4 ????93.3
??4 ????36 ????13 ????63.9 ????95.9 ????148 ??-311.1 ????97.2
??X ????94.5 ????95.7
3% carbofuran granule 2.0kg/ mu ??1 ????38 ????20 ????47.4 ????92.5 ????123 ??-223.7 ????94.8
??2 ????27 ????13 ????51.9 ????93.8 ????99 ??-266.7 ????96.5
??3 ????30 ????14 ????53.3 ????92.2 ????187 ??-523.3 ????96.9
??4 ????32 ????15 ????53.1 ????94.7 ????109 ??-240.6 ????97.7
??X ????93.3 ????95.0
Blank ??1 ????30 ????210 ????-600 ?????- ????1870 ??-6133.3 ?????-
??2 ????33 ????256 ????-675.8 ?????- ????3420 ??-10263.6 ?????-
??3 ????39 ????234 ????-500 ?????- ????2450 ??-6182.1 ?????-
??4 ????31 ????275 ????-787.1 ?????- ????4610 ??-14777.1 ?????-
??- ?????- ?????-
Table 2 is respectively handled the preventive effect after 1,3,7 day and is proofreaied and correct preventive effect
Handle Repeat 7 days 15 days 30 days
The insect population rate (%) that goes down Proofread and correct preventive effect (%) The insect population rate (%) that goes down Proofread and correct preventive effect (%) The insect population rate (%) that goes down Proofread and correct preventive effect (%)
A ??1 ????-45.0 ??82.9 ??-706 ????90.4 ??-11400 ??54.8
??2 ????0 ??83.8 ??-631 ????89.9 ??-10726 ??52.1
??3 ????17.0 ??87.5 ??-750 ????89.0 ??-11267 ??56.8
??4 ????5.0 ??87.5 ??-432 ????91.9 ??-10127 ??52.7
??X ??85.8 ????90.3 ??54.1
??B ??1 ????36.0 ??92.5 ??-244 ????95.9 ??-5000 ??80.0
??2 ????58.0 ??93.2 ??-163 ????96.4 ??-4160 ??81.1
??3 ????57.0 ??93.6 ??-414 ????93.4 ??-5520 ??78.5
??4 ????55.0 ??94.2 ??-377 ????92.7 ??-4550 ??78.5
??X ??93.4 ????94.6 ??79.5
??C ??1 ????88.0 ??98.5 ??-1130 ????97.5 ??-2608 ??89.4
??2 ????84.0 ??97.4 ??-1810 ????96.1 ??-2174 ??89.9
??3 ????89.0 ??98.4 ??-2780 ????95.1 ??-3067 ??87.9
??4 ????73.0 ??96.5 ??-396 ????92.3 ??-2496 ??88.0
??X ??97.7 ????95.3 ??88.8
??D ??1 ????43.0 ??93.3 ??-211 ????96.3 ??-3300 ??86.6
??2 ????53.0 ??92.4 ??-288 ????94.6 ??-3253 ??85.2
??3 ????58.0 ??93.7 ??-343 ????94.3 ??-3275 ??87.1
??4 ????58.0 ??94.6 ??-458 ????91.5 ??-3317 ??84.2
??X ??93.5 ????94.2 ??85.8
??E ??1 ????-750 ??-8250 ??-25350
??2 ????-518 ??-7156 ??-22481
??3 ????-569 ??-7659 ??-26107
??4 ????-679 ??-6474 ??-21539
??X
??F ??1
??2
??3
??4
Table 33% carbofuran---chlorophos granule control cotten aphid weak effect opposite sex check
Handle Proofread and correct preventive effect The significance of difference
????0.05 ????0.01
????C ????95.3 ????a ????A
????B ????94.6 ????a ????A
????D ????94.2 ????a ????A
????A ????90.3 ????b ????B

Claims (8)

1, a kind of granular insecticide, its feature is carrier with sand in this granule, is 3% carbofuran and chlorophos by granule weight outsourcing gross weight, wherein carbofuran is 0.2-2.8%.
2, by the described granular insecticide of claim 1, wherein carbofuran is counted 0.5-2.5% by granule weight.
3, by the described granular insecticide of claim 1, wherein carbofuran is counted 1.0-2.0% by granule weight.
4, by each described granular insecticide among the claim 1-3, wherein near carrier sand surface, scribble polyvinyl alcohol adhesive.
5, by the described granular insecticide of claim 1, wherein the carrier fineness of sand is the 16-50 order.
6, the method for the described granular insecticide of a kind of production claim 1, this method comprises following step successively:
(1) screening and oven dry sand;
(2) with polyvinyl alcohol: alkaline crystal violet: water=1.7: 1: the 15-17 weight ratio is mixed each material, and to neutral, heating gets painted binding agent liquid, this liquid is added in the resulting sand of step (1) and with it mix with the sour solution of transferring;
(3) add the carbofuran of 0.2%-2.8% in step (2) the gained mixture by granule weight, mixing;
(4) with chlorophos: methyl alcohol=weight ratio made the chlorophos methanol solution in 3: 1, this solution was added in step (3) the gained mixture mixing;
(5) oven dry.
7, by the described production method of claim 6, wherein oven dry is what to carry out under 70-80 ℃ hot-air.
8, by of the application of described 3% carbofuran of claim 1-chlorophos granule as cotten aphid, corn borer, peanut nematode, sugarcane field tiger insecticide.
CN 98101116 1998-03-19 1998-03-19 Insecticide containing organic nitrogen and organic phosphorus compound, its prepn. method and application Pending CN1229584A (en)

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Application Number Priority Date Filing Date Title
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101999399A (en) * 2010-10-21 2011-04-06 广州甘蔗糖业研究所 Sugarcane insecticide containing neonicotinoid insecticide
CN1883263B (en) * 2005-06-23 2011-12-28 拜尔农作物科学株式会社 Mixed granular pesticide compound
CN103651522A (en) * 2013-10-31 2014-03-26 湖南农业大学 Deltamethrin or composition thereof and application in preventing plant nematodiasis
CN108601349A (en) * 2015-12-07 2018-09-28 瓦伦特生物科学有限责任公司 Gibberellin granular preparation

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1883263B (en) * 2005-06-23 2011-12-28 拜尔农作物科学株式会社 Mixed granular pesticide compound
CN102100228B (en) * 2005-06-23 2014-02-19 拜尔农作物科学株式会社 A mixed granular agricultural chemical composition
CN101999399A (en) * 2010-10-21 2011-04-06 广州甘蔗糖业研究所 Sugarcane insecticide containing neonicotinoid insecticide
CN103651522A (en) * 2013-10-31 2014-03-26 湖南农业大学 Deltamethrin or composition thereof and application in preventing plant nematodiasis
CN108601349A (en) * 2015-12-07 2018-09-28 瓦伦特生物科学有限责任公司 Gibberellin granular preparation

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