CN106818838B - Gel Holotrichia parallela gyplure sustained-release dosage type and its preparation method and application - Google Patents
Gel Holotrichia parallela gyplure sustained-release dosage type and its preparation method and application Download PDFInfo
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- CN106818838B CN106818838B CN201710033633.6A CN201710033633A CN106818838B CN 106818838 B CN106818838 B CN 106818838B CN 201710033633 A CN201710033633 A CN 201710033633A CN 106818838 B CN106818838 B CN 106818838B
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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
- A01N49/00—Biocides, pest repellants or attractants, or plant growth regulators, containing compounds containing the group, wherein m+n>=1, both X together may also mean —Y— or a direct carbon-to-carbon bond, and the carbon atoms marked with an asterisk are not part of any ring system other than that which may be formed by the atoms X, the carbon atoms in square brackets being part of any acyclic or cyclic structure, or the group, wherein A means a carbon atom or Y, n>=0, and not more than one of these carbon atoms being a member of the same ring system, e.g. juvenile insect hormones or mimics thereof
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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
- 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
- A01N25/02—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 containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
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- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
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Abstract
The present invention relates to a kind of gel Holotrichia parallela gyplure sustained-release dosage types, are mainly prepared from the following materials: gyplure effective component, sustained-release gel carrier and solvent；The mass ratio of the gyplure effective component and sustained-release gel carrier solid content is 1:0.2-0.6；The mass volume ratio of the sustained-release gel carrier solid content and solvent is 1:5-20；The gyplure effective component is the l-Isoleucine methyl esters and (R)-(-)-linalool that mass ratio is 5-7:1；The sustained-release gel carrier is the hypromellose and hydroxypropyl methylcellulose phthalate that mass ratio is 1:0.1-0.4；The solvent is the ethyl alcohol and deionized water that volume ratio is 1:10-20.The sustained release preparation lasting period of the present invention is up to 60 days, preparation process is simple, release rule is obvious, environmentally protective, and Holotrichia parallela entire adult active stage can be covered by having the characteristics that disposably to launch, conducive to being widely applied, there is apparent economic benefit and ecological significance.
Description
Technical field
The present invention relates to a kind of gyplure sustained-release dosage types and its preparation method and application, and in particular to a kind of gel is black dull
Gill cockchafer is sustained gyplure and its preparation method and application.
Background technique
Holotrichia parallela be it is a kind of be distributed very extensive agriculture and forestry pest, harmfulness occupies first of all kinds of chafers.It is black dull
1 year generation generation of gill cockchafer, at Eimeria summer generation type, the adult generally to sprout wings takes place in early and middle ten days in June, in August under
Ten days terminates.The leaves such as imago feeding elm, poplar, willow, Chinese scholartree have the characteristics that binge.It is the main feeding peanut of larva, big
Under ground portion in the various crops such as beans, potato, wheat often results in crop and drops in production over a large area and even has no harvest, therefore always worm
The emphasis of evil preventing and controlling.Simultaneously as its larva is mainly caused harm in underground, have the characteristics that concealment is strong, also gives prevention and treatment work
Bring extreme difficulties.The problems such as conventional chemical prevention and control method is easy to produce pesticide residue, environmental pollution, pest resistance to insecticide；
The drawbacks of physical controls such as insecticidal lamp method then has while killing natural enemy.In Holotrichia parallela adult active stage, usability is lured
Its adult is traped in agent, is the novel green Control Technology of a kind of " subterranean pest-insect is controlled on the ground ", is had broad application prospects.Non-
On the basis of slow-release lure (ZL201120387584.4), this seminar has developed the lasting period at 30 days with certain release again
The sustained-release dosage type (ZL201410075001.2) of rule, peasant need not go to field to replace lure daily, liberate peasant's significantly
The amount of labour reduces the cost of labor of the Prevention Technique.But the Holotrichia parallela adult main activities phase up to two months with
On, there is no the high-efficiency sustained-release dosage forms that first use can cover Holotrichia parallela entire adult active stage substantially at present.
Summary of the invention
Object of the present invention is to for insufficient present on the above-mentioned prior art, provide a kind of lasting period to cover the black dull gill substantially
Cockchafer entire adult active stage, efficient, the gel Holotrichia parallela of release according to certain rules are sustained gyplure sustained-release dosage type.
A kind of gel Holotrichia parallela gyplure sustained-release dosage type of the present invention, mainly prepared by following raw material and
At: gyplure effective component, sustained-release gel carrier and solvent；The gyplure effective component and sustained-release gel carrier solid content
Mass ratio is 1:0.2-0.6；The mass volume ratio of the sustained-release gel carrier solid content and solvent is 1:5-20；
The l-Isoleucine methyl esters and (R)-(-)-linalool that the gyplure effective component is mass ratio 5-7:1；
The sustained-release gel carrier is the hypromellose (writing a Chinese character in simplified form HPMC) and hydroxypropyl of mass ratio 1:0.1-0.4
Cellulose phthalate (writes a Chinese character in simplified form HPMCP)；
The solvent is the ethyl alcohol and deionized water of volume ratio 1:10-20.
Further, l-Isoleucine methyl esters partial size≤420 μm (40 mesh), due to fragrant with another ingredient (R)-(-)-
Both camphor tree alcohol proportional quantities difference is larger, to make the two uniformly mixing, therefore screens out the coarse powder for being not easy to mix using fine powder crossing sieve method.
Further, borer population also is lured to increase containing accounting for gross weight 0.1-0.5% flavoring apple essence in the sustained-release dosage type.
The carrier that gel Holotrichia parallela sustained release gyplure component uses in sustained-release dosage type of the present invention is hydroxypropyl first
The gel that base cellulose and hydroxypropyl methylcellulose phthalate are combined into.Hydroxypropyl methylcellulose phthalate is
Using hydroxypropyl methyl cellulose as skeleton, the product that is esterified with phthalic anhydride.HPMCP is easy to form saturation in ethyl alcohol
Matrix type gel has matrix type structure, and has good storage stability.HPMC is similarly matrix type carrier, is easy to water
Middle formation gel, but the ability of gel blocking drug that HPMC is formed in water is less than HPMCP.HPMCP forms solidifying in ethyl alcohol
It when glue, is swollen with dehydrated alcohol, higher cost.It is easily mixed with HPMC hydrogel after HPMCP forms ethyl alcohol gel, so sharp
It is covered the shortage with the advantages of the two with merging, the retardation of HPMCP can be utilized and utilizes HPMC readily soluble bulging in water
At the characteristic of gel, save the cost.Therefore, the present invention uses hydroxypropyl methylcellulose phthalate and hydroxypropyl methylcellulose
Element is used as main sustained-release gel carrier, and Holotrichia parallela sex pheromone is prepared gelled sustained-release dosage type.Using ethyl alcohol and go
The environmental protection of ionized water, low toxicity, it is cheap the advantages that, disperse sex pheromone more evenly, and discharge by certain speed, bred in adult
And it is uniformly discharged in active stage it is expected to achieve the purpose that lure worm.
It is a further object to provide the preparation sides of the gel Holotrichia parallela gyplure sustained-release dosage type
Method follows the steps below:
(1) it prepares gel carrier: the HPMC of recipe quantity and 0-10 DEG C of deionized water being mixed, and placed at 0-10 DEG C,
Until forming clear gel；The HPMCP of recipe quantity is mixed with 0-10 DEG C of dehydrated alcohol and is placed at 0-10 DEG C, until being formed
Gel is then added in HPMC gel, stirs evenly, obtains gel carrier；
(2) addition of (R)-(-)-linalool: recipe quantity (R)-(-)-linalool is weighed, gel carrier is progressively increased with equivalent
Mode be added thereto, stir evenly；
(3) addition of l-Isoleucine methyl esters: the mixed gel that l-Isoleucine methyl esters and step (2) are obtained is sufficiently mixed
Stir well it is even, until forming uniform mixture；
(4) acquisition of sustained-release dosage type: the mixture that step (3) is obtained stands 2h or more, if gel is not stratified, explanation
Sustained-release dosage type is successfully prepared, spare.
Wherein, in step (1) HPMC and HPMCP be all 0-10 DEG C at a temperature of be swollen, at such a temperature with protect
Hinder it to be sufficiently swollen.
Being added at one time in step (2) using the method ratio that equivalent is progressively increased can more mix well.
For step (2), (3), since (R)-(-)-linalool in gyplure effective component is liquid, l-Isoleucine
Methyl esters is solid, and the two dosage difference is larger, therefore the two is sequentially formed gel respectively, to guarantee to be uniformly mixed.
Further, also containing gross weight 0.1-0.5% flavoring apple essence is accounted in the sustained-release dosage type, flavoring apple essence is in step
(3) it is added and mixes well afterwards.
It is a further object to provide the application of the gel Holotrichia parallela gyplure sustained-release dosage type, when
When applied to trapping Holotrichia parallela, it should be ensured that the 3.5g-30g of effective component containing gyplure, preferably 25g-30g in sustained-release dosage type.
The present invention has the advantages that
Relative to existing Holotrichia parallela gyplure dosage form, the present invention prepares gel using novel auxiliary material HPMCP and HPMC
Shape sustained-release dosage type, except have many advantages, such as dosage save reliable, release rule is obvious, it is environmentally protective in addition to, can be used as disposably makes
With the high-efficiency sustained-release dosage form that can cover Holotrichia parallela entire adult active stage substantially, the trapping of Holotrichia parallela is acted on
Effect is for 60 days, the shortcomings that overcoming short existing dosage form lasting period, waste of manpower cost.The preparation process of dosage form of the present invention
Simply, packing is convenient, and the feasibility with large-scale production is conducive to large-scale promotion, has apparent economic significance and life
State meaning.
Detailed description of the invention
Fig. 1 is that flavoring apple essence unites on the comparison that crop field lures worm to influence in Holotrichia parallela gyplure sustained-release dosage type of the present invention
Meter；
Fig. 2 is that the Holotrichia parallela gel gyplure crop field of various dose of the present invention lures worm effect contrast figure；
Fig. 3 is the release profiles of Holotrichia parallela gyplure sustained-release dosage type of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, right below in conjunction with drawings and examples
The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.
Embodiment 1-4 carries out ingredient according to table 1, and follows the steps below preparation.
1 embodiment 1-4 list of ingredients of table
By the component of embodiment 1-4, step prepares gel rubber sustained-release dosage form in accordance with the following methods:
(1) it ingredient: is weighed according to table 1 or measures each component: wherein partial size≤420um (40 of l-Isoleucine methyl esters
Mesh)；
(2) it prepares gel carrier: HPMC and 0-10 DEG C of deionized water being mixed, and placed at 0-10 DEG C, until being formed
Clear gel；HPMCP is mixed with 0-10 DEG C of dehydrated alcohol and is placed at 0-10 DEG C, until forming gel, is then added to
It in HPMC gel, stirs evenly, obtains gel carrier；
(3) addition of (R)-(-)-linalool: recipe quantity (R)-(-)-linalool is weighed, gel carrier is progressively increased with equivalent
Mode be added thereto, stir evenly；
(4) addition of l-Isoleucine methyl esters: the mixed gel that l-Isoleucine methyl esters and step (3) are obtained is sufficiently mixed
Stir well it is even, until forming uniform mixture；
(5) acquisition of sustained-release dosage type: the gel products that step (4) is obtained place 2h, after determining that gel layering does not occur,
Loaded on spare in bottle.
Particularly, flavoring apple essence is added in step (3) in embodiment 4 afterwards, stirs evenly, then carries out step (4).
The present embodiment 1-4 gel Holotrichia parallela gyplure sustained-release dosage type field trap effect: in 2016 6 to August
Part, crop field trapping experiments are carried out in Shandong Peanut Inst., experimental plot, Laixi.Using sustained-release dosage type made from embodiment 1-4 as
Experimental group, the content of gyplure effective component are respectively 3.5g, 25g, 30g, 25g.It is conventional degreasing with non-time-release type lure
Cotton lure as control, the control lure each contain 2ml concentration be 180mg/ml Holotrichia parallela sex pheromone effectively at
Point.3 repetitions of experimental setup.60 meters of spacing between trapper.To guarantee the trap effect of control lure every night more during test
The control lure renewed is placed into the collecting bag of every trapper before 7 points at dusk；Gel Holotrichia parallela gyplure is slow
Release dosage form is no longer replaced after being placed in field.The borer population lured in each trapper is recorded in investigation every night.
It can be obtained by Fig. 1 and Fig. 2, this gel Holotrichia parallela sustained release gyplure lures worm to work well, and lures the worm lasting period can
Up to 60 days or more.Borer population amount is lured to be higher than the prescription that flavoring apple essence is not added after flavoring apple essence is added.
5 gel Holotrichia parallela sustained release gyplure laboratory slow release effect researchs of embodiment:
The sustained release preparation prepared in embodiment 2 is placed under natural conditions and is discharged, every 5 days recycling samples, utilization is ultraviolet
Spectrophotometry measures the residual volume of gyplure effective component, obtains the releasing curve diagram (Fig. 3) of its residual volume and time relationship.By
Fig. 3 can be obtained, and in 65 days, residual volume and time are in second degree trinomial expression rule relationship, release profiles y=0.0086x2-
1.4182x+77.969 R2=0.9955.And at the 65th day, the residual volume of gyplure effective component still has 20%, about 5g, foot
Enough satisfactions lure worm demand.
Above embodiment, which is intended to illustrate the present invention, to be realized or use for professional and technical personnel in the field, therefore this hair
It is bright include but is not limited to above embodiment, it is any meet the claims or specification description, meet with it is disclosed herein
Principle and novelty, the method for inventive features, technique, product, fall within the scope of protection of the present invention.
Claims (7)
1. a kind of gel Holotrichia parallela gyplure sustained-release dosage type, which is characterized in that be mainly prepared from the following materials: property
Lure effective component, sustained-release gel carrier and solvent；The quality of the gyplure effective component and sustained-release gel carrier solid content
Than for 1:0.2-0.6；The mass volume ratio of the sustained-release gel carrier solid content and solvent is 1:5-20；
The l-Isoleucine methyl esters and (R)-(-)-linalool that the gyplure effective component is mass ratio 5-7:1；
The sustained-release gel carrier is the hypromellose and hypromellose O-phthalic of mass ratio 1:0.1-0.4
Acid esters；
The solvent is the ethyl alcohol and deionized water of volume ratio 1:10-20.
2. gel Holotrichia parallela gyplure sustained-release dosage type according to claim 1, which is characterized in that the sustained release agent
Also containing the flavoring apple essence for accounting for gross weight 0.1-0.5% in type.
3. gel Holotrichia parallela gyplure sustained-release dosage type according to claim 1 or 2, which is characterized in that the L-
Isoleucine methyl ester partial size≤420 μm.
4. the preparation method of any gel Holotrichia parallela gyplure sustained-release dosage type of claim 1-3, which is characterized in that
It follows the steps below:
(1) it prepares gel carrier: the HPMC of recipe quantity and 0-10 DEG C of deionized water being mixed, and placed at 0-10 DEG C, until
Form clear gel；The HPMCP of recipe quantity is mixed with 0-10 DEG C of dehydrated alcohol and is placed at 0-10 DEG C, until being formed solidifying
Glue is then added in HPMC gel, stirs evenly, obtains gel carrier；
(2) addition of linalool: weighing recipe quantity (R)-(-)-linalool, and gel carrier is added in such a way that equivalent is progressively increased
Wherein, it stirs evenly；
(3) addition of l-Isoleucine methyl esters: the abundant puddling of mixed gel that l-Isoleucine methyl esters and step (2) are obtained is equal
It is even, until forming uniform mixture；
(4) acquisition of sustained-release dosage type: the mixture that step (3) obtains is stood into 2h or more and illustrates to be sustained if gel is not stratified
Dosage form is successfully prepared, spare.
5. the preparation method according to claim 4, which is characterized in that also contain in the sustained-release dosage type and account for gross weight 0.1-
0.5% flavoring apple essence, flavoring apple essence are added and mix well afterwards in step (3).
6. the application of any gel Holotrichia parallela gyplure sustained-release dosage type of claim 1-3, which is characterized in that when answering
When for traping Holotrichia parallela, it should be ensured that the 3.5g-30g of effective component containing gyplure in sustained-release dosage type.
7. application according to claim 6, which is characterized in that the 25g-30g of effective component containing gyplure in sustained-release dosage type.
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| CN201710033633.6A CN106818838B (en) | 2017-01-17 | 2017-01-17 | Gel Holotrichia parallela gyplure sustained-release dosage type and its preparation method and application |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108552207A (en) * | 2018-05-21 | 2018-09-21 | 山东省花生研究所 | A kind of trans- Synergistic slow release gelling agent of Holotrichia parallela first and its preparation and effect |
| CN108684671A (en) * | 2018-05-21 | 2018-10-23 | 山东省花生研究所 | A kind of cis- Synergistic slow release gelling agent of Holotrichia parallela first and its preparation and effect |
| CN109793011A (en) * | 2018-12-29 | 2019-05-24 | 广州瑞丰生物科技有限公司 | A kind of longicorn attractant and preparation method |
| CN109907040A (en) * | 2019-04-12 | 2019-06-21 | 浙江省食品药品检验研究院 | A kind of sustained-release gel ball and preparation method thereof with controlling plant diseases function |
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| CN101502491A (en) * | 2009-03-09 | 2009-08-12 | 山东省医药工业研究所 | Dirithromycin enteric-coated formulation |
| CN101627757A (en) * | 2009-08-03 | 2010-01-20 | 山东省花生研究所 | Dark melolonthidae sex pheromone and sex attractant |
| CN103828808A (en) * | 2014-03-03 | 2014-06-04 | 山东省花生研究所 | Pasty Holotrichia parallela sex attractant sustained-release preparation and preparation method thereof |
| CN104041490A (en) * | 2014-06-13 | 2014-09-17 | 山东省花生研究所 | Granular holotrichia parallela slow-releasing sex attractant and preparation method thereof |
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2017
- 2017-01-17 CN CN201710033633.6A patent/CN106818838B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101502491A (en) * | 2009-03-09 | 2009-08-12 | 山东省医药工业研究所 | Dirithromycin enteric-coated formulation |
| CN101627757A (en) * | 2009-08-03 | 2010-01-20 | 山东省花生研究所 | Dark melolonthidae sex pheromone and sex attractant |
| CN103828808A (en) * | 2014-03-03 | 2014-06-04 | 山东省花生研究所 | Pasty Holotrichia parallela sex attractant sustained-release preparation and preparation method thereof |
| CN104041490A (en) * | 2014-06-13 | 2014-09-17 | 山东省花生研究所 | Granular holotrichia parallela slow-releasing sex attractant and preparation method thereof |
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Effective date of registration: 20221212 Address after: Room 211, Block D, Lanhua Institute, No. 36, Jinshui Road, Laoshan District, Qingdao City, Shandong Province, 266000 Patentee after: QINGDAO RUSSELL IPM BIOTECH CO.,LTD. Address before: Licang District 266000 years Springs Road No. 126, Shandong city of Qingdao Province Patentee before: SHANDONG PEANUT Research Institute |