CN106665645A - Refined trichlorfon composition and preparation method and application thereof - Google Patents
Refined trichlorfon composition and preparation method and application thereof Download PDFInfo
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- CN106665645A CN106665645A CN201611199419.XA CN201611199419A CN106665645A CN 106665645 A CN106665645 A CN 106665645A CN 201611199419 A CN201611199419 A CN 201611199419A CN 106665645 A CN106665645 A CN 106665645A
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- composition
- refining dipterex
- tablet
- dipterex
- refining
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds
- A01N57/20—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds containing acyclic or cycloaliphatic radicals
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/66—Phosphorus compounds
- A61K31/662—Phosphorus acids or esters thereof having P—C bonds, e.g. foscarnet, trichlorfon
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/20—Pills, tablets, discs, rods
- A61K9/2004—Excipients; Inactive ingredients
- A61K9/2022—Organic macromolecular compounds
- A61K9/205—Polysaccharides, e.g. alginate, gums; Cyclodextrin
- A61K9/2059—Starch, including chemically or physically modified derivatives; Amylose; Amylopectin; Dextrin
Abstract
The invention belongs to the technical field of pesticide preparations, particularly relates to a refined trichlorfon composition, and further discloses a preparation method and application of the refined trichlorfon composition. The refined trichlorfon composition comprises a refined trichlorfon crude medicine, a compound enzyme agent and a functional additive at the mass ratio of 100:(0.5-3):(2-5). According to the refined trichlorfon composition, the refined trichlorfon crude medicine is taken as an effective ingredient, and the auxiliary effects of the compound enzyme agent and the functional additive are added, so that the insect repellent effect of the trichlorfon crude medicine is further strengthened, parasites of fecal egg infection or visceral parasite infection can be effectively eliminated by a refined trichlorfon tablet; above all, a higher insect repellent effect can be obtained by the trichlorfon tablet under the condition of a lower effective dose and the effective repellent rate is close to 100%.
Description
Technical field
The invention belongs to technical field of pesticide preparations, and in particular to a kind of refining dipterex composition, and further disclose
Its preparation method and application.
Background technology
Metrifonate, scientific name O, O- dimethyl-(2,2,2- tri- chloro- 1- hydroxyethyls) phosphonate ester, Chinese nickname includes enemy hundred
Worm soluble powder, metrifonate are for animals, trichlorphon original powder, dimethyl-(the chloro- 1- hydroxyethyls of 2,2,2- tri-) phosphate, refined
Metrifonate etc..Metrifonate is a kind of organophosphorus insecticide, and its industrial products is white solid, molecular weight 257.43, sterling fusing point
83-84 DEG C, density 1.73 (20 DEG C), 10% aqueous solution index of refraction is 1.3439, the μ Pa of vapour pressure 7.8 (20 DEG C).Metrifonate has
There is aromatic odor, water and organic solvent can be dissolved in, 100 milliliters of 15.4 grams of water dissolvables at 25 DEG C, and as temperature is raised, enemy
Solubility increase of hundred worms in water.Metrifonate property is relatively stablized, but chance alkali is then hydrolyzed into DDVP, and acute toxicity LD50 values are
Big white mouse is orally 560~630mg/kg.
Metrifonate belongs to one kind of organophosphorus pesticide-phosphate type, and hydroxyl replaces shape by organic group in phosphoric acid molecules
Compound into phosphorus carbon key turns into phosphoric acid, and phosphoric acid is esterified as phosphate, and acceptable daily intake is 0.01mg/ (kg.d),
The toxicity of metrifonate is based on acute poisoning, and slow poisoning is smaller.Metrifonate is relatively stablized in acid and neutral solution, in alkalescence
Under the conditions of easily decompose and lose toxicity, but product DDVP can be obtained after metrifonate is decomposed in the basic conditions, increase its toxicity
It is big 10 times.
The Main Function of metrifonate is used as insecticide, is a kind of organophosphorus insecticide, with efficient, low toxicity, low
The characteristics of residual, it is a kind of broad spectrum insecticide.Metrifonate has action of contace poison concurrently based on stomach poison function, also there is osmotically active,
It is parasitic suitable for the pests with chewing mouthparts on the crops such as water paddy and wheat class, vegetables, tea tree, fruit tree, mulberry tree, cotton, and domestic animal
Worm, the preventing and treating of sanitary insect pest.Metrifonate is also very wide in agriculturally range of application, can be used to prevent and treat cabbage caterpillar, Amrasca biguttula (Ishida), Sang Ye
The preventing and treating of the various pests such as silkworm, Phellinus, weevil, fruit tree sawfly, fruit bat；Can also be used for treating snail fever, be in herding
A kind of good multiple-effect pest repellant.
Trichlorphon original powder can be processed into the various formulations such as pulvis, wettable powder, soluble powder and emulsion and use, and also may be used
Direct obtained aqueous solution is made poison bait, agriculture, woods, gardening pest insect for preventing and treating biting mouthparts and sucking mouth parts, underground
Insect etc.；Also after can be by the refined purification processes of active compound, for preventing and treating epizoa in pig, ox, horse, mule livestock body, to family and
Public health insect is effective.
The content of the invention
Therefore, the technical problems to be solved by the invention are to provide a kind of refining dipterex composition, further to carry
The desinsection drug effect of refining dipterex high.
In order to solve the above technical problems, refining dipterex composition of the present invention, including mass ratio is 100：0.5-
3：The refining dipterex active compound of 2-5, complex enzyme agent and functional additive.
Preferably, the mass ratio of the refining dipterex active compound, complex enzyme agent and functional additive is 100：1.5：3.
The complex enzyme agent is selected from the mixture of one or more in phytase, beta-lactamase or lysozyme, and excellent
Select three's mixed in equal amounts.
The functional additive is selected from the mixture of one or more in hyaluronic acid, polyglutamic acid or trehalose, and
It is preferred that three's mixed in equal amounts.
The method of described refining dipterex composition is prepared the invention also discloses a kind of, including is taken a selected amount of described
Refining dipterex active compound, complex enzyme agent and functional additive, and the step of mixed.
Obtained in as described refining dipterex composition addition customary adjuvant, according to common process
Metrifonate preparation.
It is conventional auxiliary by described refining dipterex composition addition the invention also discloses a kind of refining dipterex tablet
Material, according to tablet obtained in common process.
Preferably, the preparing raw material of the tablet includes：
More excellent, the preparing raw material of the tablet includes：
The invention also discloses a kind of method for preparing described refining dipterex tablet, comprise the following steps：
(1) get the raw materials ready：Take a selected amount of starch and add water and be made starch slurry, it is standby；
(2) softwood：A selected amount of refining dipterex active compound and calcium monohydrogen phosphate are taken, trough-type mixture machine stirring is sequentially added, and
Add starch slurry to stir and evenly mix, be made softwood；
(3) pelletize：Gained softwood is pelletized according to common process, dry and whole grain treatment, and by whole grain after
Grain adds a selected amount of hard magnesium to mix；
(4) compressing tablet：Above-mentioned particle is carried out into compressing tablet, is obtained final product.
It is used to prepare the purposes of metrifonate insecticidal preparation the invention also discloses described refining dipterex composition.
The insecticide is parasite insecticide for animals, including endoparasite and vermin are specifically, described
Insecticide is used to drive away domestic animal gastrointestinal nematode parasites, pig fasciolopsis, bot, warble, sheep nose fly maggot and tick, mite, flea, lice
Deng parasite.
The insecticidal preparation is for oral administration, and a secondary amounts is every 1Kg body weight, horse 30-50mg, ox 20-40mg, sheep 80-
100mg, goat 50-70mg, pig 80-100mg.
Refining dipterex composition of the present invention, with refining dipterex active compound as active ingredient, its expelling parasite principle with enemy
Hundred worms are approximate, and it is combined with the cholinesterase of polypide, suppress the activity of cholinesterase, acetylcholine is largely accumulated, and disturb worm
The nervimuscular neuromuscular juinction of body, causes sensitive parasite to be benumbed and dead.And in addition complex enzyme agent and functional additive
Booster action, the anthelminthic effect of trichlorfon technical is further enhancing, either for the infection of faecal egg, or internal organ
The desinsection of the infection conditions of parasite, refining dipterex tablet of the present invention can effectively be driven away；Importantly, this
Inventing the metrifonate tablet can obtain anthelminthic effect higher under lower effective dose addition, and effective purge ratio connects
Nearly 100%.
Specific embodiment
Refining dipterex active compound of the present invention is the commercially available refining dipterex active compound powder of prior art, also can be according to existing
Have purification technique known to technology carries out refinement treatment and obtains to trichlorfon technical, and such as Chinese patent CN 102234292B are public
A kind of metrifonate purifying technique is opened.The refining dipterex active compound being related in following embodiments is to implement according to above-mentioned patent document
Method is obtained in example 2.
The refining dipterex tablet of embodiment 1
Refining dipterex composition described in the present embodiment includes that mass ratio is 100：1.5：It is 3 refining dipterex active compound, multiple
Synthase agent and functional additive.
The complex enzyme agent is phytase, beta-lactamase and lysozyme with 1：1：1 mass ratio mixing.
The functional additive is hyaluronic acid, polyglutamic acid and trehalose with 1：1：1 mass ratio mixing.
Refining dipterex tablet has the following raw material to prepare described in the present embodiment：
The method that the present embodiment prepares described refining dipterex tablet, comprises the following steps：
(1) get the raw materials ready：Take a selected amount of starch and add water and be made the starch slurry of about 14wt%, it is standby；
(2) softwood：A selected amount of refining dipterex active compound and calcium monohydrogen phosphate are taken, trough-type mixture machine is sequentially added and is stirred 15 points
Clock, and add starch slurry (being cooled to less than 40 DEG C) to stir and evenly mix 10 minutes, it is made softwood；
(3) pelletize：Using oscillating granulator, the granulation of 12 mesh sieves is crossed, the particle that will be prepared is placed in basin, is controlled
Wet grain is thick to be no more than 1.5cm, in 40 DEG C of aeration-dryings；Period, up to 30 minutes stirrings first of temperature, rear every 20 minutes stirrings are once simultaneously
Record；Dried particle is crossed into 14 mesh sieve whole grains, control powder is about 3 with particle fraction：7, add V-type to mix whole good particle
A selected amount of hard magnesium is added in conjunction machine, is mixed 10 minutes；
(4) compressing tablet：Add the tablet press machine hopper to carry out compressing tablet appropriate above-mentioned particle, and coupon weight, hardness, thickness, collapse
Xie Du, friability and outward appearance, obtain final product.
The refining dipterex tablet of embodiment 2
Refining dipterex composition described in the present embodiment includes that mass ratio is 100：3：It is 2 refining dipterex active compound, compound
Enzyme agent and functional additive.
The complex enzyme agent is phytase, beta-lactamase and lysozyme with 1：1：1 mass ratio mixing.
The functional additive is hyaluronic acid, polyglutamic acid and trehalose with 1：1：1 mass ratio mixing.
Refining dipterex tablet has the following raw material to prepare described in the present embodiment：
The method that the present embodiment prepares described refining dipterex tablet is same as Example 1.
The refining dipterex tablet of embodiment 3
Refining dipterex composition described in the present embodiment includes that mass ratio is 100：0.5：It is 2 refining dipterex active compound, multiple
Synthase agent and functional additive.
The complex enzyme agent is phytase, beta-lactamase and lysozyme with 1：1：1 mass ratio mixing.
The functional additive is hyaluronic acid, polyglutamic acid and trehalose with 1：1：1 mass ratio mixing.
Refining dipterex tablet has the following raw material to prepare described in the present embodiment：
The method that the present embodiment prepares described refining dipterex tablet is same as Example 1.
The refining dipterex tablet of embodiment 4
The preparing raw material and ratio of refining dipterex tablet described in the present embodiment are same as Example 1, and it is differed only in,
The refining dipterex composition includes that mass ratio is 100：1.5：3 refining dipterex active compound, phytase and polyglutamic acid.
The refining dipterex tablet of embodiment 5
The preparing raw material and ratio of refining dipterex tablet described in the present embodiment are same as Example 1, and it is differed only in,
The refining dipterex composition includes that mass ratio is 100：1.5：3 refining dipterex active compound, beta-lactamase and transparent
Matter acid.
The refining dipterex tablet of embodiment 6
The preparing raw material and ratio of refining dipterex tablet described in the present embodiment are same as Example 1, and it is differed only in,
The refining dipterex composition includes that mass ratio is 100：1.5：3 refining dipterex active compound, lysozyme and trehalose.
Comparative example 1
The preparing raw material and ratio of refining dipterex tablet described in this comparative example are same as Example 1, and it is differed only in,
The refining dipterex composition includes that mass ratio is 100：4.5 refining dipterex active compound and complex enzyme agent.
The complex enzyme agent is phytase, beta-lactamase and lysozyme with 1：1：1 mass ratio mixing.
Comparative example 2
The preparing raw material and ratio of refining dipterex tablet described in this comparative example are same as Example 1, and it is differed only in,
The refining dipterex composition includes that mass ratio is 100：4.5 refining dipterex active compound and functional additive.
The functional additive is hyaluronic acid, polyglutamic acid and trehalose with 1：1：1 mass ratio mixing.
Experimental example
1.1 material
Obtained refining dipterex tablet in embodiment 1-6 and comparative example 1-2, and be right with existing refining dipterex active compound
As usual.
Experimental animal：300 bi-crossbreedings of 5 months ages in days raised to certain pig farm, carry out pig parasitic ovum excrement
Check, and do record in detail, 100 more serious pigs of selection infection are randomly divided into 10 groups, every group 10, carry out mark, carry out
Experiment.
1.2 methods and result
Test pig Investigation On Parasitic Infections：One group of 10 test pig is taken before experiment to butcher, and carries out Fasciola hepatica, silk ribbon
The inspection of worm, gastrointestinal nematode and other parasitic infection amounts.Determine this area's pig main parasitic worm Mean abund ance.
Other 9 groups of experiments are applied into refining dipterex tablet in embodiment 1-6, comparative example 1-2 with pig respectively, and with refined
Trichlorfon technical is control, is calculated according to every kg body weight administration 100mg preparations of pig, twice daily, orally.
The faecal egg inspection of each group test pig, observation infection worm are carried out with McMaster methods after being administered 7,14,21 days
Ovum reduces situation, and Redution of eggs is calculated by following equation, and experimental result see the table below 1：
The faecal egg infective dose alimentary canal worm's ovum amount of table 1 reduces situation
Each experimental animal Mean abund ance change before and after experiment：Total Test pig send slaughterhouse to be slaughtered after off-test
Kill, and collect the inspection that internal organ do Fasciola hepatica, tapeworm, gastrointestinal nematode and other parasitic infection amounts.Before determining experiment
The situation of change of each group Mean abund ance afterwards, deworming rates are calculated by following equation, and each parasite expelling parasite situation is recorded in
Table 2 below：
Each parasite of table 2 tests forward backward averaging infection intensity situation of change (deworming rates %)
| Numbering | Fasciola hepatica deworming rates/% | Tapeworm deworming rates/% | Gastrointestinal nematode parasites deworming rates/% |
| Embodiment 1 | 99.2% | 99% | 99.5% |
| Embodiment 2 | 99% | 99.1% | 99.2% |
| Embodiment 3 | 99.3% | 99% | 99.1% |
| Embodiment 4 | 97.9% | 98.2% | 98.1% |
| Embodiment 5 | 98.1% | 98.2% | 98.0% |
| Embodiment 6 | 97.9% | 98.1% | 97.9% |
| Comparative example 1 | 71.2% | 70.8% | 70.1% |
| Comparative example 2 | 70.9% | 71.1% | 70.8% |
| Reference examples | 70.3% | 71.3% | 71.2% |
Can be seen that infection either for faecal egg from upper table data, or internal organ parasite infection conditions
Desinsection, refining dipterex tablet of the present invention can effectively drive away, and effective purge ratio is close to 100%.In addition, from upper
Table data are it can also be seen that individually add the preparation of complex enzyme agent or functional additive, its anthelminthic effect opposes hundred with exclusive use
The effect of worm active compound is suitable, it is contemplated that above-mentioned experiment is the refined enemy hundred of the present invention in the case of identical medicament applied amount
Worm tablet is even more in the case of relatively low effective dose, further improves anthelminthic effect.
Obviously, above-described embodiment is only intended to clearly illustrate example, and not to the restriction of implementation method.It is right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need and unable to be exhaustive to all of implementation method.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. a kind of refining dipterex composition, it is characterised in that including mass ratio be 100：0.5-3：The refining dipterex of 2-5 is former
Medicine, complex enzyme agent and functional additive.
2. refining dipterex composition according to claim 1, it is characterised in that the complex enzyme agent be selected from phytase,
The mixture of one or more in beta-lactamase or lysozyme.
3. refining dipterex composition according to claim 1 and 2, it is characterised in that the functional additive is selected from saturating
The mixture of one or more in bright matter acid, polyglutamic acid or trehalose.
4. a kind of method for preparing the refining dipterex composition described in claim any one of 1-3, it is characterised in that including taking
The a selected amount of refining dipterex active compound, complex enzyme agent and functional additive, and the step of mixed.
5. the refining dipterex composition as described in claim any one of 1-3 adds customary adjuvant, is obtained according to common process
Metrifonate preparation.
6. a kind of refining dipterex tablet, it is characterised in that the refining dipterex composition as described in claim any one of 1-3
Addition customary adjuvant, according to tablet obtained in common process.
7. refining dipterex tablet according to claim 6, it is characterised in that the preparing raw material of the tablet includes：
8. a kind of method of the refining dipterex tablet prepared described in claim 7, it is characterised in that comprise the following steps：
(1) get the raw materials ready：Take a selected amount of starch and add water and be made starch slurry, it is standby；
(2) softwood：A selected amount of refining dipterex active compound and calcium monohydrogen phosphate are taken, trough-type mixture machine stirring is sequentially added, and add
Starch slurry is stirred and evenly mixed, and is made softwood；
(3) pelletize：Gained softwood is pelletized according to common process, is dried and whole grain treatment, and the particle after whole grain is added
Enter a selected amount of hard magnesium to mix；
(4) compressing tablet：Above-mentioned particle is carried out into compressing tablet, is obtained final product.
9. the refining dipterex composition described in any one of claim 1-3 is used to prepare the use of metrifonate insecticidal preparation or agricultural chemicals
On the way.
10. purposes according to claim 9, it is characterised in that the insecticide is parasite insecticide for animals.
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| CN201611199419.XA CN106665645B (en) | 2016-12-22 | 2016-12-22 | A kind of refining dipterex composition and the preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611199419.XA CN106665645B (en) | 2016-12-22 | 2016-12-22 | A kind of refining dipterex composition and the preparation method and application thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1220874A (en) * | 1997-10-27 | 1999-06-30 | Ss制药株式会社 | Drug composition with controlled drug release rate |
| CN101934070A (en) * | 2009-07-02 | 2011-01-05 | 天津瑞普生物技术股份有限公司 | Veterinary antibacterial drug composition containing lysozyme and oligosaccharide and application thereof |
| CN104337822A (en) * | 2013-07-25 | 2015-02-11 | 青岛康地恩动物药业有限公司 | Compound tablets containing mebendazole and dipterex and used for deworming on pets, and preparation method thereof |
-
2016
- 2016-12-22 CN CN201611199419.XA patent/CN106665645B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1220874A (en) * | 1997-10-27 | 1999-06-30 | Ss制药株式会社 | Drug composition with controlled drug release rate |
| CN101934070A (en) * | 2009-07-02 | 2011-01-05 | 天津瑞普生物技术股份有限公司 | Veterinary antibacterial drug composition containing lysozyme and oligosaccharide and application thereof |
| CN104337822A (en) * | 2013-07-25 | 2015-02-11 | 青岛康地恩动物药业有限公司 | Compound tablets containing mebendazole and dipterex and used for deworming on pets, and preparation method thereof |
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| CN106665645B (en) | 2019-08-27 |
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Address after: 253100 Eastern District, Pingyuan County Economic Development Zone, Dezhou City, Shandong Province Applicant after: Dezhou Jingxin Pharmaceutical Co., Ltd. Address before: 253100 Eastern District, Pingyuan County Economic Development Zone, Dezhou City, Shandong Province Applicant before: Dezhou Jingxin Pharmaceutical Co., Ltd. |
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Denomination of invention: The invention relates to a refined trichlorfon composition and a preparation method and application thereof Effective date of registration: 20210914 Granted publication date: 20190827 Pledgee: Pingyuan County sub branch of Postal Savings Bank of China Ltd. Pledgor: Dezhou Jingxin Pharmaceutical Co.,Ltd. Registration number: Y2021980009326 |
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