CN1109708A - Plant pesticide composition and preparing process thereof - Google Patents
Plant pesticide composition and preparing process thereof Download PDFInfo
- Publication number
- CN1109708A CN1109708A CN94109325A CN94109325A CN1109708A CN 1109708 A CN1109708 A CN 1109708A CN 94109325 A CN94109325 A CN 94109325A CN 94109325 A CN94109325 A CN 94109325A CN 1109708 A CN1109708 A CN 1109708A
- Authority
- CN
- China
- Prior art keywords
- plant pesticide
- pesticide composition
- plant
- tobacco
- solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The plant composition as pesticide is prepared with extract liquid from 8 Chinese medicinal materials such as flavescent sophora root, tobacco, Sichuan aconite root, trichosanthes fruit, etc., compounded with emulsifier, adhesive and solvent through mixing them together, and features low cost and toxicity, broad-spectrum effect, and synergistic function.
Description
The present invention relates to a kind of is the composition pesticide and preparation method thereof of primary raw material with the plant extraction liquid, and particularly a kind of is composition pesticide of primary raw material and preparation method thereof with kuh-seng, tobacco extract.
At present, green tide extend over the entire globe, countries in the world have given great attention to the protection of ecotope.Because the population growth ploughs and reduces relatively, for satisfying the basic living necessities of people, effective control of damage by disease and insect becomes the output of assurance agricultural product and the necessary condition of quality.Yet, for a long time, because a large amount of chemical pesticides that use, not only caused pollution to ecotope, also make some sick worm produce resistance to a certain degree, cause the chemical pesticide consumption further to increase, incidents such as the agricultural byproducts of chemical pesticide pollution simultaneously, underground water happen occasionally, to the threat to a certain degree of mankind's formation.Development and utilization more and more is subjected to the attention of various countries to environment and human harmless agricultural chemicals resource own.
Show that according to documents and materials a lot of countries are all at the research botanical pesticide.Plant insecticide activity and effective ingredient thereof have been carried out comparatively deep research.People such as Lshida have carried out the eastern subterranean termite antifeedant activity is studied with 11 kinds of chemical compositions of the methanol extraction thing of neem oil.R.Nakatani etc. and Muangi, studied the compound of several trichilin of the being called A-F that contain in the rhizome of francolin Pittosporum (Trichilia) plant, these compounds are effective food refusal effects of spodoptera, mexican bean ladybird, and the real noctuid of tobacco budworm, fall army worm and paddy is also had the growth inhibition effect.People such as Kraug isolate two kinds of tetracyclic triterpenoids from Australian Chinese toon, they claim that these two kinds of compounds are toonacilin and 6-acetoxytoonacilin.These compounds demonstrate very strong antifeedant activity and contact toxicity to mexican bean ladybird.Find successively that in the plant of cloud spices some have the chemical substance of insecticidal activity, these materials comprise gedunin, bussein, entanrophragmin, nomilin, cedrelone and anthothecol.People such as Arnason have assessed their activity to corn borer etc.The ethereal extract of research such as Jacobson U.S. Echinacea plant finds that it has toxic effect to mosquito larvae, housefly, and yellow mealworm and danaus plexippus worm are also had the growth inhibition effect, its active ingredient is accredited as N-isobutyl-E2, E6, E8, E10-dodecatetraenamide.People such as Pirman are isolated alatoctone from native Chinese toon, and the confused flour beetle insect is had killing action.Juvocimene-L that people such as Bowers extract from hair sweet basil leaf and Juvocimene-II have juvenile hormone activity to the Ursula butterfly worm, and the culex larva is also had stronger killing action.People such as Simmonds isolate the diterpene-kind compound of number of C lerodane from cadbait, and find that they have antifeedant activity to the larva of extra large spodoptera and cotton bollworm.People such as Klocke have studied Rhododendron molle, and separating the composition of providing activity from it is spent is rhodojaronin III, grayanatoxin III and Kalmanol, and they demonstrate food refusal, growth inhibition and cytotoxicity to the larva of colorado potato beetles, fall army worm.Also have from Milan in addition, plant extract separating effective ingredients such as citrus oils, Shi Kuju, carpet bugle, nine flavors, one skill wormwood artemisia, sweetsop, lily magnolia, Psoralea corylifolia, and certain effect is arranged all.International in a word work is to separate, to be extracted as the master, and is not many to the repercussion study between each plant species.
In recent years, done a series of activities aspect the botanical pesticide that China has been known very early at pyrethrin, nicotine, rotenone etc., developed some products, as pyrethrin, nicotine sulphate, derris extract etc.Also on some other plant, do a lot simultaneously, new discovery is also arranged.Zhao is kind, and joyous the grade once systematically introduced toosendanin and nimbin to neurotoxicity and food refusal effects such as corn borer, diamond-back moths.Liang Xiaotian etc. identified to its structure once that Liu Zhun etc. had carried out the structure evaluation to the novel substance-rhodojaponin V that has insecticidal activity in chrysanthemum, the cuckoo (Rhododenclronmolle).Liu Zhun etc. also are reported in and have four kinds of alkaloids and four kinds of limonin substances in shaggy-fruited dittany (Dictamnus dasycarpus) root.Wherein dictamine (Dictamine) all has different bacteriostatic activities with 8-hydroxyl dictamine (8-hydroxy dictamine) to 14 plant species fungies such as cercospora leaf spot of sugar beet.Li Zhengming etc. once identified 27 kinds of trace organic substances from the plant of Solanaceae lilac, find that wherein the acetate leaf-alcohol has the activity that good avoiding keeps away mosquito.The report that also has the root of langdu, the tuber of stemona, fennel artemisin etc.
The purpose of this invention is to provide a kind of plant pesticide composition and method of making the same.
Another object of the present invention provides that a kind of cost is low, the plant pesticide composition and method of making the same of low toxicity.
Plant pesticide composition of the present invention be with kuh-seng, tobacco, monkshood, radix aconiti agrestis, melon wither, Li Lu, the root of langdu and thunder godvine eight plant species are raw material, after pulverizing lixiviate, leaching liquor and emulsifier, spreader-sticker and solvent are mixed and make, described solvent is an ethanol.Described pesticide combination composition formula is: shrubby sophora extract is 0.3～1.2%, tobacco extract is 0.1～0.2%, monkshood, radix aconiti agrestis, melon withers, Li Lu, the root of langdu and triperygium wilfordii extractive are respectively 0.05～0.02%, described extract is with soluble solids juice in the extract, emulsifier is 7～8%, spreader-sticker is 2～3%, above percentage all calculates with the plant pesticide composition total weight, emulsifier wherein, spreader-sticker is used emulsifier and a spreader-sticker in the prior art, surplus is a solvent, described solvent is generally the second alcohol and water, also can be any a kind of solvent or mixed solvent that is suitable for above-mentioned each component is made into stable liquid.Described plant pesticide composition pH value is adjusted to 3～6, and preferred pH value is 4～4.5.When water content in the described composition pesticide during greater than 10 weight %, said composition is easy to decompose and lost efficacy in preparation with when storing, and therefore, water content should≤10% in the plant pesticide composition of the present invention.
Plant pesticide composition of the present invention prepares from the following stated scheme.
1, kuh-seng, tobacco, monkshood, radix aconiti agrestis, melon are withered, Li Lu, the root of langdu and thunder godvine pulverize respectively, be suitable for lixiviate and be as the criterion to be crushed to.
2, wherein kuh-seng, monkshood, radix aconiti agrestis, melon wither, Li Lu, the root of langdu and thunder godvine crushed material be respectively with the solvent lixiviate, and described solvent is an alcohols, for example methyl alcohol, ethanol, dimethylbenzene or acetone.The solvent for use amount is in the lixiviate groove, and solvent can flood extract and be as the criterion, and extraction temperature is a room temperature, and extraction time is 7～10 days, filters separation then, collects filtrate.
The used extraction solvent of tobacco is 5～10% limewash for the lime weight percentage, and other lixiviate step is the same.Isolated by filtration filtrate transfers to pH value 3～7 with acid, and used acid can be hydrochloric acid or sulfuric acid.
3, above-mentioned leaching liquor is mixed, adds emulsifier, spreader-sticker and etoh solvent simultaneously, and product P H value is transferred to 3～6, preferred pH value 4～4.5, control product moisture content is less than or equal to 10 weight %, obtains plant pesticide composition of the present invention.
Wherein each active princlple addition adds by the control of quantitative chemical analysis means, and moisture control is quoted GB600-chemical titration (karl-Fischer method) and measured and control.PH value is measured and is quoted GB1601-agricultural chemicals method for hydrogen ion concentration mensuration.Emulsion stability is measured and is quoted GB1603-pesticidal emulsifiable stability determination method.
Plant pesticide of the present invention belongs to low-toxin farm chemicals, plant pesticide acute toxicity experience of the present invention is shown, to mouse per os LD50 great and mighty or powerful is 2330(1600～3390) mg/Kg, to female rat through skin LD50＞200mg/Kg, the result shows, according to China's agricultural chemicals acute toxicity grading criteria, plant pesticide per os of the present invention and all belong to low-toxin farm chemicals through the skin acute toxicity.
Indoor and field control effectiveness test evaluation:
When plant pesticide composition of the present invention according to surveying and determination dilutes 1000 times, prevent and treat 24 hours effects 100% of 3 cotton bollworms in age, still reach 96% when diluting 3000 times, dilute 500 times to 4～5 age cotton bollworm preventive effect 86.7%, 24 hours preventive effects were 77.8% when cotten aphid was diluted 1000 times, and 24 hours preventive effects reached 100% when cotten aphid was diluted 1000 times.Dilute 1000 times and soak leaf, the diamond-back moth lethality is that the calibration lethality is 92.3% after 76.7%, 48 hour after 24 hours.Dilute the preventive effect of 1000 times of liquid to black peach aphid, after the dispenser 1st be 95.8%, 3 be 94.1%, 5 day be 90.0%.Above laboratory test all shows, plant pesticide composition of the present invention is good to control cotton bollworm, diamond-back moth, black peach aphid drug effect.
Field control effectiveness test in Hebei, ground such as Jiangsu, Hubei mainly prevent and kill off the test of object cotton bollworm, three ground synthesis result, 500 times of 5 days preventive effects of plant pesticide composition dilution of the present invention are about 85%, dilute 1000 times of 5 days preventive effects more than 80%, and the test of pesticide effectiveness is all carried out in the high resistance helicoverpa armigera district, effect is good, is considered to one of good pharmacopoeia that prevents and treats cotton bollworm.
Toxicity Determination to plant pesticide composition of the present invention shows, plant pesticide composition of the present invention has good malicious valency effect to cotton bollworm, (Ji County, Hebei insecticide factory produces its virulence for contrast medicament 40% nuvacron missible oil, commercially available) 11.02 times of virulence, Toxicity Determination has synergistic effect to cotton bollworm co-toxicity coefficient 167.
It is extensive that plant pesticide of the present invention and preparation method thereof has raw material sources, and the industrial production three-waste free discharge itself is difficult for producing contamination accident, and cost is lower than advantages such as chemical pesticide commonly used, because of natural goods easily is degraded, environmental protection is played a role.
Further specify the present invention by the following examples.
Embodiment 1:
Get 600 kilograms of kuh-sengs, tobacco 120 kg, 50 kilograms of monkshoods, 50 kilograms of radix aconiti agrestis, melon wither 50 kilograms, 50 kilograms of Li Lu, 50 kilograms of the roots of langdu, 30 kilograms of thunder godvines, pulverize respectively, be respectively charged in the lixiviate groove, wherein contain adding 7% limewash in the tobacco groove, other each groove adds ethanol lixiviate, and the extraction solvent addition was not as the criterion there not to be material, lixiviate is 8 days under the room temperature, filter respectively then, collect filtrate, the tobacco leaching liquor transfers to PH5.2 with hydrochloric acid.
By shrubby sophora extract content 0.7%, tobacco extract 0.2%, monkshood, radix aconiti agrestis, melon wither, Li Lu, the root of langdu and triperygium wilfordii extractive be respectively the 0.03% above-mentioned leaching liquor that is mixed, add 7% emulsifier and 2% spreader-sticker simultaneously, surplus is an etoh solvent, and PH transfers to 4.5 with mixed liquor, makes product.
Embodiment 2:
With embodiment 1, wherein the used extraction solvent of tobacco is 10% limewash, and other uses dimethylbenzene, lixiviate 10 days, and the finished product pH value transfers to 6.
Embodiment 3:
With embodiment 1, wherein the used extraction solvent of tobacco is 5% limewash, and other uses acetone, lixiviate 7 days.
By shrubby sophora extract 1.2%, tobacco extract 0.1%, monkshood extract be 0.05%, radix aconiti agrestis, melon wither, Li Lu, the root of langdu and triperygium wilfordii extractive are respectively 0.02% and are mixed, and add 8% emulsifier simultaneously, 3% spreader-sticker, surplus is an ethanol, mixed liquor PH transfers to 3.
Embodiment 4:
With embodiment 2, wherein the finished product pH value transfers to 4.5.
Embodiment 5:
With embodiment 3, wherein other uses extraction solvent to be methyl alcohol except that tobacco, lixiviate 9 days.
Embodiment 6:
With embodiment 3, wherein by shrubby sophora extract 0.3%, tobacco extract 0.2%, monkshood, radix aconiti agrestis, melon wither, Li Lu, the root of langdu and triperygium wilfordii extractive be respectively 0.02% and be mixed, and adds 7% emulsifier and 3% spreader-sticker simultaneously, surplus is an ethanol, PH transfers to 5.5 with mixed liquor, makes product.
Claims (10)
1, a kind of plant pesticide composition, it is characterized in that be by kuh-seng, tobacco, monkshood, radix aconiti agrestis, melon wither, Li Lu, the root of langdu and thunder godvine leaching liquor and emulsifier, spreader-sticker and solvent be mixed and make.
2, plant pesticide composition according to claim 1, it is characterized in that shrubby sophora extract is 0.3～1.2%, tobacco extract is 0.1～0.2%, monkshood, radix aconiti agrestis, melon wither, Li Lu, the root of langdu and triperygium wilfordii extractive are respectively 0.05～0.02%, described extract is with soluble solids juice in the extract, and emulsifier is 7～8%, and spreader-sticker is 2～3%, above percentage all calculates with the plant pesticide composition total weight, and surplus is an etoh solvent.
3, plant pesticide composition as claimed in claim 1 or 2 is characterized in that described plant pesticide composition pH value transfers to 3～6.
4, as plant pesticide composition as described in the claim 3, it is characterized in that described plant pesticide composition pH value to 4～4.5.
5, plant pesticide composition as claimed in claim 1 or 2 is characterized in that described plant pesticide composition comprises water amount≤10%.
6, a kind of plant pesticide preparation of compositions method, it is characterized in that with kuh-seng, monkshood, radix aconiti agrestis, melon wither, Li Lu, the root of langdu and thunder godvine pulverize respectively; With the solvent lixiviate, described solvent is an alcohols respectively, comprises methyl alcohol, ethanol, dimethylbenzene or acetone; Extraction temperature is a room temperature, extraction time 7～10 days, and isolated by filtration is collected filtrate then; Tobacco is used 5～10 weight % limewash lixiviates after crushed, and room temperature lixiviate 7～10 days is filtered then and transferred to PH3～7 with acid, collects filtrate; To collect filtrate being mixed, add emulsifier, spreader-sticker and etoh solvent simultaneously, make the plant pesticide product.
7, as plant pesticide preparation of compositions method as described in the claim 6, it is characterized in that controlling product water content≤10 weight %.
8, as plant pesticide preparation of compositions method as described in claim 6 or 7, it is characterized in that product P H value transfers to 3～6.
9, as plant pesticide preparation of compositions method as described in claim 6 or 7, it is characterized in that product P H value transfers to 4～4.5.
10,, it is characterized in that tobacco leaching liquor PH regulates acid and is hydrochloric acid or sulfuric acid as plant pesticide preparation of compositions method as described in the claim 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94109325A CN1109708A (en) | 1994-12-28 | 1994-12-28 | Plant pesticide composition and preparing process thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94109325A CN1109708A (en) | 1994-12-28 | 1994-12-28 | Plant pesticide composition and preparing process thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1109708A true CN1109708A (en) | 1995-10-11 |
Family
ID=5033868
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94109325A Pending CN1109708A (en) | 1994-12-28 | 1994-12-28 | Plant pesticide composition and preparing process thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1109708A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101843267A (en) * | 2010-05-20 | 2010-09-29 | 北京绿神保科技有限公司 | High-efficiency nontoxic insecticide and preparation method thereof |
| CN101156609B (en) * | 2007-11-20 | 2010-11-24 | 史建生 | A plant pesticide including matrine and its preparing method as well as application |
| CN101156607B (en) * | 2007-11-20 | 2010-11-24 | 史建生 | A plant pesticide and its preparing method as well as application |
| CN102960371A (en) * | 2012-12-18 | 2013-03-13 | 江苏省中国科学院植物研究所 | Application of radix trichosanthis water extract to biological pesticides |
| CN103242085A (en) * | 2012-04-18 | 2013-08-14 | 湖北省文东农业发展有限公司 | Organic plant foliar fertilizer and preparation and spraying methods of organic plant foliar fertilizer |
| CN105532764A (en) * | 2016-02-17 | 2016-05-04 | 广西大学 | Environmentally-friendly botanical pesticide and preparation method thereof |
| CN106332907A (en) * | 2016-08-19 | 2017-01-18 | 浙江师范大学 | Preparation method of trchosahthes kirilowii maxin pulp natural preservative |
| CN106508996A (en) * | 2016-10-31 | 2017-03-22 | 郑州思辩科技有限公司 | Greenhouse pesticide and preparation method thereof |
| CN109805042A (en) * | 2019-03-04 | 2019-05-28 | 邯郸市建华植物农药厂 | A kind of killing aphids aqua and its production technology containing jervine |
| CN112314635A (en) * | 2020-10-30 | 2021-02-05 | 柳州衍生科技有限公司 | Insecticide containing silkworm chrysalis powder and preparation method thereof |
-
1994
- 1994-12-28 CN CN94109325A patent/CN1109708A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101156609B (en) * | 2007-11-20 | 2010-11-24 | 史建生 | A plant pesticide including matrine and its preparing method as well as application |
| CN101156607B (en) * | 2007-11-20 | 2010-11-24 | 史建生 | A plant pesticide and its preparing method as well as application |
| CN101843267A (en) * | 2010-05-20 | 2010-09-29 | 北京绿神保科技有限公司 | High-efficiency nontoxic insecticide and preparation method thereof |
| CN103242085A (en) * | 2012-04-18 | 2013-08-14 | 湖北省文东农业发展有限公司 | Organic plant foliar fertilizer and preparation and spraying methods of organic plant foliar fertilizer |
| CN102960371A (en) * | 2012-12-18 | 2013-03-13 | 江苏省中国科学院植物研究所 | Application of radix trichosanthis water extract to biological pesticides |
| CN105532764A (en) * | 2016-02-17 | 2016-05-04 | 广西大学 | Environmentally-friendly botanical pesticide and preparation method thereof |
| CN106332907A (en) * | 2016-08-19 | 2017-01-18 | 浙江师范大学 | Preparation method of trchosahthes kirilowii maxin pulp natural preservative |
| CN106508996A (en) * | 2016-10-31 | 2017-03-22 | 郑州思辩科技有限公司 | Greenhouse pesticide and preparation method thereof |
| CN109805042A (en) * | 2019-03-04 | 2019-05-28 | 邯郸市建华植物农药厂 | A kind of killing aphids aqua and its production technology containing jervine |
| CN112314635A (en) * | 2020-10-30 | 2021-02-05 | 柳州衍生科技有限公司 | Insecticide containing silkworm chrysalis powder and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Bekele et al. | Evaluation of Ocimum kenyense (Ayobangira) as source of repellents, toxicants and protectants in storage against three major stored product insect pests | |
| Oyedokun et al. | Pesticidal efficacy of three tropical herbal plants' leaf extracts against Macrotermes bellicosus, an emerging pest of cocoa, Theobroma cacao L. | |
| Edwin et al. | Bioinsecticidal potency of five plant extracts against cowpea weevil, Callosobruchus maculatus (F.), on stored cowpea, Vigna unguiculata (L) | |
| Oparaeke et al. | Evaluation of botanical mixtures for insect pests management on cowpea plants | |
| Rao et al. | Evaluation of neem, Azadirachta indica, with and without water management, for the control of culicine mosquito larvae in rice‐fields | |
| CN1109708A (en) | Plant pesticide composition and preparing process thereof | |
| CN101069508A (en) | Farm chemical composition, preparing method and use | |
| CN1826905A (en) | Compound pesticide of triperygium wilfordii alkaloid | |
| CN101919403A (en) | Pesticide composition of allyl isothiocyanate and phoxim | |
| Chiu | Effectiveness of Chinese insecticidal plants with reference to the comparative toxicity of botanical and synthetic insecticides | |
| CN105123700A (en) | Insecticidal and bactericidal agent with thymol and arecoline and preparation method of insecticidal and bactericidal agent | |
| CN110973164A (en) | Ginkgolic acid soluble solution and preparation method thereof | |
| Aditama et al. | Optimizing of maseration with ethanol and water solvents against the toxicity of extract of wuluh starfruit (Averrhoa bilimbi L.) in controlling larva of Aedes aegypti. | |
| CN105532680B (en) | A kind of highly efficiency compositional composition pesticide of pyrimidine containing trifluoro-benzene and cycloxaprid | |
| Byers et al. | Residues on coastal bermudagrass, trash, and soil treated with granular endosulfan | |
| CN103271081B (en) | Etoxazole-triazophospesticide pesticide composition | |
| CN111357777A (en) | Deinsectization ovum-inhibiting agent extracted from plant containing sweet wormwood herb and preparation and application methods thereof | |
| Ogunleye | Toxicity bioassays of four different botanicals against the house hold pest: Periplaneta americana (Linnaeus) | |
| Saradamma | Biological activity of different plant extracts with particular reference to their insecticidal, hormonal and antifee ding actions | |
| KR101740270B1 (en) | A fast-acting natural insecticidal composition containing plant extract as an active component and manufacturing method of the same | |
| Christian et al. | The effect of three plants aqueous extracts on feed intake and reproduction parameters of Coelaenomenodera lameensis Berti and Mariau (Coleoptera: Chrysomelidae) the pest of oil palm | |
| CN101006793A (en) | A nuisance-free botanical insecticides preparation process | |
| CN104381320A (en) | Non-polluted pesticide adopting camphor tree leaves as raw materials | |
| CN105284910A (en) | Pesticide prepared from loose knot | |
| EP0591674A2 (en) | Use of meliaceae plants or parts of these plants as plant protecting agent with fungicidal activity |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination |