CN101142913A - Avermectin nanometer medicine-carried system with slow-releasing and controlled-releasing action - Google Patents
Avermectin nanometer medicine-carried system with slow-releasing and controlled-releasing action Download PDFInfo
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Abstract
The invention relates to an avermectin water dispersible granule (WG) nano drug-loaded system which is prepared by mixing, grinding and granulation of reasonable proportion of a dispersant, a disintegrating agent, a filling material and an avermectin nano drug-loaded particle. The avermectin nano drug-loaded particle is formed after a nano silica carrying material with porous structure effectively carries a pesticide active ingredient of avermectin with physical absorption. The avermectin nano drug-loaded system appears like a cylinder-shaped particle and automatically disperses and forms suspension in water when in use, moreover, the invention has significant slow and controlled release effect on the avermectin and can also effectively reduce hydrolysis and photolysis of the avermectin in water solution.
Description
Technical field
The present invention relates to a kind of nanometer silicon dioxide material and effectively carry the avermectin nanometer medicine-carried particle that forms after the pesticide active ingredient Avermectin by physisorption with loose structure, with rational proportion and dispersant, disintegrant and filler through Avermectin water dispersible granules (WG) nanometer medicine-carried system that mixes, pulverizing, granulation form.Belong to pesticidal preparations and learn research field, rate of release, the hydrolysis that slows down Avermectin and the photodissociation after the major control Avermectin is used, the safety in increasing operation rate, increase preparation processing and using.
Background technology
The proposition of nineteen ninety nanometer technology (nano scale technology), research provides a kind of thinking different with traditional sense and method with biological medicine for life science.In the medical research field, nanometer technology is used for drug research and exploitation, preparation or synthetic new Nano medication, overcome the limitation that conventional medicament toxic and side effect in clinical practice is strong, bioavilability is low, realized that controlled delivery of pharmaceutical agents discharges and the target transmission, promote the revolution of modern pharmacology research and drug manufacture, promoted the formation that modern pharmacology research field new discipline-Nano medication is learned.
In the pesticidal preparations research field, the formulations of pesticide are the important means that realize the transmission of pesticide active ingredient effective dose, improve chemistry security, determined to a great extent agricultural chemical compound to the biologically active of control target, to the mankind's safety and with the compatibility of environment.Along with the attention of the enhancing of human environment protection consciousness, food security and rural laborer continuous increase to aspect pressure such as cities and towns transfers, make improve the agricultural chemicals availability, increase the agricultural chemicals safety in utilization, to prolong the cry of agricultural chemicals lasting period more surging., be a kind of biopesticide that meets world's agricultural chemicals development trend and CHINESE INDUSTRIES policy particularly for efficient, broad-spectrum biological source pesticide kinds such as Avermectin.Now, China has become the main manufacture base of world's Avermectin, spreads all over the product that the accumulative total registration of national 400 many enterprises contains Avermectin and reaches more than 1000, and former medicine production scaleization, preparation formulation are various, have become domestic main pesticide species.But there are problems such as easily degraded, lasting period lack in the use, the agricultural chemicals availability is low in Avermectin to water, photaesthesia.By formulation processing alleviate its preparation processing and use in organic solvent, dust etc. to operator's harm, reduce photodissociation, hydrolysis equistability problem that preparation uses back active ingredient, realize that its sustained release under effective biological dose is significant.
At present, 200510125988.5) and long-acting slow-release oil suspending agent (Chinese patent application number: 200510125989.X) formulation of commercialization pesticide avermectin mainly contains missible oil, wetting powder, microcapsule suspending agent etc., and bibliographical information or the formulation of having applied for patent of invention have nano-microcapsule suspending agent (Chinese patent: X03121410), long-effective slow-release wetable powder (Chinese patent application number:.Graininess water dispersible granules (WG) the nanometer medicine-carried system patent of invention with slow-releasing and controlled-releasing action at the Avermectin research and development yet there are no report at home and abroad.
At this present situation, we utilize the acquired achievement of Nano medication school work, in conjunction with the key technical problem that exists in the pesticide science use, researched and developed a kind of graininess water dispersible granules (WG) nanometer medicine-carried system that Avermectin is had slow-releasing and controlled-releasing action, this medicine-carried system outward appearance is a cylindrical pellet, and spontaneous dispersion forms suspension to water during use.Through the indoor and outdoor evidence, this medicine-carried system is guaranteeing under the prerequisite of effective biological dose Avermectin to be had tangible slow-releasing and controlled-releasing action, makes it the lasting period obviously to extend, improved the agricultural chemicals availability, reduced environmental pollution, reduced spraying times, reduced labour intensity.This has very important Science ﹠ Society meaning undoubtedly.
Summary of the invention
The objective of the invention is to release rate of release, the hydrolysis that slows down Avermectin and photodissociation after a kind of controlled Avermectin is used, a kind of Avermectin graininess water dispersible granules (WG) nanometer medicine-carried system (hereinafter to be referred as avermectin nanometer medicine-carried system) of the safety in increasing operation rate, increase preparation processing and using with slow-releasing and controlled-releasing action, thereby improve the agricultural chemicals availability, reduce environmental pollution, reduce spraying times, reduce labour intensity, realize the sustainable development of the formulations of pesticide.
To achieve these objectives, 1. the present invention selects to take formulation as the leading factor with missible oil, wetting powder at present, and the biogenic pesticide Avermectin that occupation rate of market is big, development prospect is wide is a pesticide active ingredient.Through formulation optimization, raising preparation processing and safety in utilization, can produce the economy and society benefit rapidly.At present, the research report that does not also have this respect.2. adopt a kind of nanometer silicon dioxide material with loose structure, effectively carry by physisorption and to form avermectin nanometer medicine-carried particle after the Avermectin, production technology is simple, load-carrying efficiency is high, stable performance, can realize rapidly that industrialization transforms.3. according to present China formulations of pesticide current situation, the extruder grain method that finally adopts medicine-carried system is processed into cylindric water dispersible granules (WG) formulation, mature production technology does not need the investment that increases manufacturing facilities in addition on existing water dispersible granules (WG) formulation processing basis.
The technical solution used in the present invention is: a kind of avermectin nanometer medicine-carried system with slow-releasing and controlled-releasing action is characterized in that: 1. pesticide active ingredient is Avermectin (English general abamectin by name), and best effectively working concentration is 1～20%; 2. carrier material is a kind of nano silicon with loose structure, can effectively carry by physisorption and form avermectin nanometer medicine-carried particle after the Avermectin, and its bearing capacity to Avermectin is 10～80% of an own wt; 3. the dispersant of Shi Yonging is one or two a mixture in anion surfactant sodium lignin sulfonate, naphthalenesulfonate formaldehyde condensation compound, the polymethylacrylic acid carboxylate graft copolymer, and weight percentage is 1～10%6; 4. the disintegrant of Shi Yonging is the mixture of ammonium sulfate, soluble starch, one or more filler of sodium carboxymethylcellulose, and weight percentage is 1～10%; 5. the filler of Shi Yonging is the mixture of one or more filler in white carbon, bentonite, the diatomite, and weight percentage is 10～80%; 6. medicine-carried system finally is processed into water dispersible granules (WG) formulation, and outward appearance is a cylindrical pellet, and spontaneous dispersion forms suspension to water during use.7. the medicine-carried system hybrid mode is agravic mixing, and grinding mode is a comminution by gas stream, and the granulation mode is an extruder grain.
Wherein, the avermectin nanometer medicine-carried system with slow-releasing and controlled-releasing action of the present invention, the pesticide active ingredient that is carried is an Avermectin, its weight percentage in medicine-carried system is 1～20%.Used carrier is the nano silicon with loose structure, average grain diameter 100～500nm, form avermectin nanometer medicine-carried particle with Avermectin by physisorption, wherein Avermectin is 10～80% of a nanometer silicon dioxide material own wt.The dispersant that uses is one or two a mixture in anion surfactant sodium lignin sulfonate, naphthalenesulfonate formaldehyde condensation compound, the polymethylacrylic acid carboxylate graft copolymer, and weight percentage is 1～10%.The disintegrant that uses is the mixture of ammonium sulfate, soluble starch, one or more filler of sodium carboxymethylcellulose, and weight percentage is 1～10%.The filler that uses is the mixture of one or more filler in white carbon, bentonite, the diatomite, and weight percentage is 10～80%.
The preparation method of avermectin nanometer medicine-carried system of the present invention is, at first Avermectin and the nano silicon with loose structure are formed avermectin nanometer medicine-carried particle by physisorption, take by weighing by formula rate with dispersant, disintegrant, filler etc. again, add in the agravic blender and mix, carry out comminution by gas stream, reach extruder grain after the fineness of regulation.Final pesticide water dispersible granules (WG) formulation that forms, outward appearance is a cylindrical pellet, spontaneous dispersion forms suspension to water during use.
According to the regulation of relevant agricultural chemicals national standard of China or industry standard, the avermectin nanometer medicine-carried system that the present invention develops has been carried out main performance index mensuration in indoor and outdoor.Gather as follows.
1. the pay(useful) load efficiency analysis of Avermectin
Existing at present national standard (the former medicine of Avermectin: GB 19336-2003 of Avermectin Determination on content; Abamectin emulsifiable concentrate: GB 19337-2003), but the nano silicon with loose structure does not appear in the newspapers as yet by the extracting method that physisorption forms Avermectin in the avermectin nanometer medicine-carried particle (hereinafter to be referred as avermectin nanometer medicine-carried particle).This method is exactly on existing literature method basis, formulates in conjunction with the preparation actual conditions.
Concrete operation method is as follows: accurately take by weighing sample, add quantitative organic solvent ultrasonic dissolution 10min in ultrasonic cleaner, take out centrifugal (3000r/min) 15min, filter; Accurately pipette ormal weight organic facies filtrate again and in volumetric flask, use constant volume, mix the back and measure the Avermectin effective content according to GB 19337-2003 prescriptive procedure.
In order to check the usefulness of the extracting method of Avermectin in the avermectin nanometer medicine-carried particle, also carried out the variation test of the screening of best organic solvent, different ultrasonic time Avermectin stripping quantities and method accuracy, precision determination test, the result proves that this method of inspection is effective.
Test data is as follows:
Best organic solvent The selection result sees Table 1.
Different ultrasonic time Avermectin stripping quantity result of the tests see Table 2.
The accuracy test of assay method the results are shown in Table 3.
The Precision test result of assay method sees Table 4.
Table 1 organic solvent The selection result table
| Sample/solvent | Avermectin concentration (μ g/mL) | Chromatogram response (A) | ||
| Ultrasonic 5min | Ultrasonic 10min | Ultrasonic 12min | ||
| 1. standard items/carrene | 319.5 | 7987.44 | 7817.14 | |
| 2. standard items/methyl alcohol | 349.5 | 8746.28 | 8315.29 | |
| 3. GR/ carrene | 328.8 | 8006.99 | 825?3.66 | 805?3.66 |
| 4. GR/ methyl alcohol | 358.6 | 8033.50 | 8445.42 | 8513.12 |
| 5. GR/ standard hard water | 309.8 | 114.33 | 127.85 | 135.81 |
| 6. GR/ carrene+standard hard water | 315.6 | 7458.35 | 7839.04 | 7803.04 |
Annotate: GR is avermectin nanometer medicine-carried particle in the table, and is as follows
By table 1 as seen, the Avermectin standard items, no matter carrene, methyl alcohol, ultrasonic dissolution 5min is higher than 10min chromatogram response, and difference is little between the solvent; But the dissolution efficiency carrene for Avermectin in the water dispersible granules obviously is better than methyl alcohol.
The different ultrasonic time Avermectin of table 2 stripping quantity result of the test table
| Sample/solvent | Chromatogram response (A) | ||||
| Ultrasonic 5min | Ultrasonic 10min | Ultrasonic 20min | Ultrasonic 30min | Ultrasonic 40min | |
| The GR/ carrene | 7368.16 | 7464.32 | 7419.30 | 7305.34 | 7241.24 |
| GR/ carrene+standard hard water | 6784.67 | 6882.46 | 6850.55 | 6783.27 | 6701.61 |
By table 2 as seen, the ultrasonic dissolution different time, the Avermectin stripping quantity is different.Handle 5min, 10min, 20min, 30min, 40min relatively for two of GR, Avermectin stripping concentration is the highest during 10min.
The accuracy test of table 3 assay method is table as a result
| Add concentration (μ g/ml) | 50.5 | 50.2 | 50.6 | 50.9 | 50.3 | 50.5 |
| Measure concentration (μ g/ml) | 50.3 | 49.8 | 50.2 | 50.9 | 49.8 | 50.2 |
| The rate of recovery (%) | 99.6 | 99.2 | 99.2 | 100.0 | 99.0 | 99.4 |
| Average recovery rate (%) | 99.4 | |||||
The Precision test result table of table 4 assay method
| Sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | Mean value (%) | S | CV(％) |
| Measurement result | 3.52 | 3.57 | 3.53 | 3.53 | 3.56 | 3.48 | 3.66 | 3.54 | 0.04 | 1.13 |
Show that by table 3, table 4 result method is accurately and reliably.
According to above definite test method, detect nano silicon respectively to the pay(useful) load efficient of Avermectin the weight ratio of the former medicine of Avermectin and carrier material in the avermectin nanometer medicine-carried particle (analyze), testing result sees Table 5.
Table 5 Avermectin pay(useful) load efficient testing result table
| Batch | 1 | 2 | 3 | Mean value |
| Measurement result (%) | 68.12 | 55.97 | 68.15 | 64.08 |
The result shows nano silicon energy pay(useful) load Avermectin, the weight ratio of former medicine of Avermectin and carrier material in institute's analytic sample〉50%.
2. the detection of the main physicochemical property technical indicator of avermectin nanometer medicine-carried system
At the test specimen of 5 different batches preparing respectively, adopt the method for quality control of determining that product is carried out every technical indicator and measure (measurement result sees Table 6).According to measurement result, determined the control project indicator of this product in conjunction with China's pesticide water dispersible granules correlated quality standard.
The 3.5% avermectin nanometer medicine-carried system control project indicator sees Table 7.
Table 65 batch different material source preparation sample technical indicator measured result
| Lot number | Avermectin content (%) | Outward appearance | Moisture (%) | The pH value | Fineness (%) | Suspensibility (%) | The heat storage stability test | |
| Resolution ratio (%) | Other indexs | |||||||
| 1 | 3.52 | Qualified | 1.1 | 6.2 | 97 | 85.2 | 4.5?3 | Qualified |
| 2 | 3.56 | Qualified | 2.6 | 7.0 | 92 | 78.6 | 6.76 | Qualified |
| 3 | 3.59 | Qualified | 2.0 | 6.6 | 93 | 80.3 | 5.28 | Qualified |
| 4 | 3.51 | Qualified | 2.3 | 6.8 | 95 | 83.1 | 6.09 | Qualified |
| 5 | 3.57 | Qualified | 2.2 | 7.0 | 95 | 81.6 | 6.57 | Qualified |
The table 7 3.5% avermectin nanometer medicine-carried system control project indicator
| Project | Index |
| Avermectin content, % 〉= | 3.5 |
| Moisture, %≤ | 3.0 |
| PH value scope (1% aqueous dispersions) | 5～8 |
| Fineness (by the 44um testing sieve), % 〉= | 95 |
| Wetting time, S≤ | 60 |
| Suspensibility, % 〉= | 80 |
| Heat storage stability 1) | Qualified |
| Annotate: be the pattern Interventions Requested 1), during ordinary production, the every three months check once at least. | |
3. the indoor biologically active report of accessment and test of avermectin nanometer medicine-carried system
At the slowly-releasing behavior of 3.5% avermectin nanometer medicine-carried system,,, and, carry out the indoor bioassay test at following three kinds of different Avermectin formulations for the field practical application provides theoretical foundation in order to verify its insecticidal action.
Reagent agent: 1.8% abamectin emulsifiable concentrate (being called for short EC in the table), 1.8% avermectin micro-emulsion (being called for short ME in the table), 3.5% avermectin nanometer medicine-carried system (being called for short WDG in the table).
For trying object: diamondback moth larvae.Pick up from vegetables field, Beijing, raise at indoor rape leaf, the raising condition is a room temperature (27 ± 1) ℃, and humidity is 80%, and intensity of illumination is 20001ux, and light application time is 12h every day.(weight range is that every 5.71mg～0.11mg) carries out the medicament toxicity test with 3 instar larvaes.
Toxicity test method: adopt the blade medicine embrane method to carry out toxicity test.Compare with methods such as drop method, dip methods, the advantage of blade medicine embrane method is more to approach insect and the interactional situation of agricultural chemicals under the field medication condition, also is the method that extensively adopts both at home and abroad at present.The pesticidal preparations water of different dosage form is mixed with 4
-Measure concentration for 5, concrete test concentrations sees Table 1.If clear water is a blank.Rape leave is used flushing with clean water earlier, dry, break into the small pieces that diameter is 15mm with card punch then, in soup, flood 10s, dry, it is put in 24 holes cultivates in the box every hole a slice.Diamond-back moth 3 instar larvaes are inserted be placed with in the 24 hole boxes of blade, 1 larva is inserted in every hole, seals fresh-keepingly with preservative film, puts into (27 ± 1) ℃ illumination box after adding a cover.Each concentration is handled 10 larvas, repeats 4～5 times.Check result behind the 72h is touched the complete reactionless death that is judged as of polypide with dialling pin.
Medicament lasting period assay method: with each formulation respectively water be mixed with 0.0078 μ g/mL and two dosage of 0.0625 μ g/mL, after under indoor conditions, placing 0,3,5,7 day, measure the activity of each dosage respectively by " toxicity test method " to diamond-back moth, with blank calculation correction lethality, to compare the lasting period of different dosage form.
The Avermectin different dosage form the results are shown in Table 8 to the toxicity test of diamond-back moth.
Table 8 Avermectin different dosage form is to the toxicity test (corrected mortality) of diamond-back moth
| Medicament | WDG | ME | EC |
| 0.03125μg/mL | 73.9％ | 75％ | 75％ |
| 0.062?5μg/mL | 87.5％ | 81.8％ | 82.6％ |
| 0.125μg/mL | 94.4％ | 91.6％ | 91.7％ |
| 0.25μg/mL | 100％ | 94.4％ | 100％ |
| Toxicity regression formula (Y=) | 8.75?31+2.2259x | 7.2569+1.1220x | 8.0125+1.6757x |
| LC50 value and 95% confidence limit (μ g/mL) | 0.0206 (0.00692～0.061?3) | 0.00974 (0.0005?06～0.188) | 0.01593 (0.00327～0.0776) |
| LC90 value (μ g/ml) | 0.07769 | 0.1?356 | 0.0929 |
From table 8 measurement result, though Avermectin different dosage form LC5.Value is not quite similar, but because 3 kinds of formulation LC5.95% confidence limit of value is overlapped, therefore judges that there is not significant difference in different dosage form to the virulence of diamond-back moth, and promptly virulence is in same level.
Table 9 Avermectin different dosage form to lasting period of diamond-back moth (corrected mortality, %)
| Soup standing time | 0.0078μg/mL | 0.0625μg/mL | ||||
| WDG | ME | EC | WDG | ME | EC | |
| 0 day | / | / | / | 87.5 | 81.8 | 82.6 |
| 3 days | 70.0 | 60.0 | 50.0 | 90.0 | 80.0 | 80.0 |
| 5 days | 42.1* | 31.6 | 26.3 | 73.7* | 47.4 | 47.4 |
| 7 days | 27.8* | 0 | 0 | 61.1* | 5.6 | 5.6 |
*: the different dosage form comparing difference is (p=0.05) significantly
The result finds out from table 9, and the corrected mortality basically identical of measuring when 3 kinds of formulations are placed 0 and 3 day after being mixed with soup not there are differences.Soup is placed after 5 days and is measured, and compares with the same dosage form of placing 0 and 3 day, and certain decline has appearred in the corrected mortality of avermectin nanometer medicine-carried system, but tangible decline has appearred in microemulsion and missible oil.Relatively, avermectin nanometer medicine-carried system is significantly better than latter two formulation between different dosage form.The soup of preparation was placed after 7 days, two dosage of microemulsion and missible oil lose activity substantially to diamond-back moth, and the corrected mortality of avermectin nanometer medicine-carried system 0.0625 μ g/mL still can reach more than 60%, illustrates that the lasting period of this formulation obviously is longer than microemulsion and missible oil formulation.
Testing result proves that fully avermectins long-effective controlled release water dispersible granules not only has slow releasing function, and can also keep than higher insecticidal activity.
4. avermectin nanometer medicine-carried system sustained release performance and anti-hydrolysis, photodissociation effect measuring
On behalf of aqueous dispersions, 1.8% abamectin emulsifiable concentrate (being called for short EC in the table), 1.8% avermectin micro-emulsion (being called for short ME in the table), 3.5% avermectin nanometer medicine-carried system (being called for short WDG in the table) (1. be contained in the colourless transparent glass bottle, 2. represents aqueous dispersions to be contained in the Brown Glass Brown glass bottles and jars only) Avermectin rate of decay measurement result such as table 10, table 11 to aqueous dispersions in the table under natural placement condition.
Table 10 avermectin nanometer medicine-carried system sustained release performance and anti-hydrolysis, photodissociation effect measuring be table as a result
| Sample | System | Avermectin content (%) in the agent | |||||||||
| 0 day | 1 day | 2 days | 3 days | 4 days | 5 days | 6 days | 7 days | 8 days | 9 days | 10 days | |
| EC① | 2.19 | 1.58 | 0.84 | 0.44 | 0.1?3 | 0.12 | |||||
| EC② | 2.19 | 2.02 | .87 | 1.67 | 1.63 | 1.33 | 1.29 | 1.18 | 1.02 | 0.81 | 0.72 |
| ME① | 2.16 | 1.64 | 1.52 | 1.29 | 0.96 | 0.83 | 0.63 | 0.34 | 0.25 | ||
| ME② | 2.16 | 1.73 | 1.67 | 1.64 | 1.59 | 1.46 | 1.41 | 1.37 | 1.30 | 1.26 | 1.11 |
| WDG① | 3.57 | 3.31 | 2.76 | 2.67 | 2.57 | 2.56 | 2.32 | 2.21 | 2.20 | 2.14 | 2.07 |
| WDG② | 3.57 | 3.39 | 3.19 | 3.14 | 2.98 | 2.82 | 2.74 | 2.69 | 2.57 | 2.48 | 2.45 |
Table 11 avermectin nanometer medicine-carried system sustained release performance and anti-hydrolysis, photodissociation effect measuring be table (continuing) as a result
| Sample | Avermectin content (%) in the preparation | ||||||
| 11 days | 12 days | 13 days | 14 days | 15 days | 16 days | 17 days | |
| WDG① | 1.91 | 1.73 | 1.64 | 1.37 | 1.22 | 1.09 | 0.69 |
| WDG② | 2.37 | 2.27 | 2.16 | 2.09 | 2.03 | 1.96 | 1.87 |
By table 10, table 11 as seen, the preparation aqueous solution of the same race compares, and Avermectin concentration ratio Brown Glass Brown glass bottles and jars only descends fast in the colourless transparent glass bottle; Different preparations compare, and Avermectin decline is the fastest in the cream preparation aqueous dispersions, microemulsion takes second place, avermectin nanometer medicine-carried system descends the slowest.As seen, Avermectin is in the aqueous solution, and not only photodissociation also can hydrolysis, but is better than hydrolysis with photodissociation.Avermectin hydrolysis, photodissociation be all slow in the avermectin nanometer medicine-carried system aqueous dispersions, and Avermectin valid density is held time obviously than missible oil and microemulsion formulation lengthening in the preparation aqueous dispersions.
Testing result shows that avermectin nanometer medicine-carried system not only has sustained release performance preferably, and can effectively reduce the hydrolysis and the photodissociation speed of Avermectin.
5. the cost analysis of avermectin nanometer medicine-carried system report
To the comparative analysis such as the table 12 of the existing Avermectin 1.8% cream preparation cost of 3.5% avermectin nanometer medicine-carried system and market of preparation, drug effect of equal value is to such as table 13.
Table 12 producting cost accounting contrast table (by 1 ton)
| Project | Unit price (ten thousand yuan/ton) | 3.5% avermectin nanometer medicine-carried system | 1.8% missible oil | ||
| Consumption (kg) | Cost (ten thousand yuan) | Consumption (kg) | Cost (ten thousand yuan) | ||
| The former medicine of Avermectin | 1000 | 35 (foldings hundred) | 3.5 | 18 (foldings hundred) | 1.8 |
| Wetting dispersing agent | 1 | 100 | 0.1 | ||
| Emulsifier | 1.5 | 100 | 0.15 | ||
| Solvent | 0.75 | 898 | 0.674 | ||
| Filler | 0.05 | 862 | 0.043 | ||
| Processing charges | 0.12 | 0.02 | |||
| Amount to | 3.763 | 2.644 | |||
Annotate: this table is worked out the costs of production and is not comprised packing and fringe cost.
Table 13 drug effect of equal value is calculated contrast table (calculating according to the land for growing field crops conventional spray)
| Preparation | Indoor effective dose (μ g/ml) | Field commodity consumption (g/ mu) | Reagent cost (unit/mu) | Preventive effect (%) | |||
| 0h | 72h | 120h | 168h | ||||
| 3.5% avermectin nanometer medicine-carried system | 0.0078 | 1.114 | 0.042 | 70.0 | 45.0 | 35.0 | |
| 0.0625 | 8.857 | 0.333 | 87.5 | 90.0 | 75.0 | 65.0 | |
| 1.8% missible oil | 0.0078 | 2.167 | 0.057 | 50.0 | 30.0 | 10.0 | |
| 0.0625 | 17.361 | 0.459 | 82.6 | 80.0 | 50.0 | 15.0 | |
Annotate: effective content is 100 times of indoor effective dose in the commodity consumption of this table field.
By table 12, table 13 as seen, if the indoor biometrics result is calculated the land for growing field crops conventional spray, then reaching under the situation of identical preventive effect, 3.5% avermectin nanometer medicine-carried system is lower than market existing Avermectin 1.8% cream preparation control cost.
Comprehensively above result of the test is as can be seen:
1. by selecting to have the dispenser carrier of the new material of strong absorption property as pesticide avermectin, by rational load technology can obtain greater than 50% Avermectin pay(useful) load rate (weight ratio of former medicine of Avermectin and carrier material), under selected processing technology and quality control condition, can obtain having the pesticidal preparations of stabilization technique specification, and every technical indicator all meets or exceeds the regulation of China's relevant criterion.
2. Avermectin is encapsulated in 3.5% avermectin nanometer medicine-carried system of developing in this new material, obtained good slow release effect and anti-hydrolysis, photodissociation effect, it also obviously is better than existing Avermectin 1.8% cream preparation according to the control in field cost that the indoor bioassay result calculates.
Embodiment
Further specified the present invention in order to illustrate better below by embodiment.But what it should be appreciated by those skilled in the art is that the application not merely is limited to the scope of following embodiment.
Embodiment 1:
Require accurately to take by weighing avermectin nanometer medicine-carried particle (the effective load-carry duty 60% of Avermectin), sodium lignin sulfonate 100.0 grams, naphthalenesulfonate formaldehyde condensation compound 20.0 grams, soluble starch 5.0 grams, ammonium sulfate 90.0 grams that contain Avermectin 3.5 grams according to prescription, supply 1000 grams with white carbon, under agravic condition, mixed 10 minutes, pulverize with airslide disintegrating mill.It is qualified to detect every technical indicator, promptly gets 3.5% avermectin nanometer medicine-carried system.
Embodiment 2:
Require accurately to take by weighing avermectin nanometer medicine-carried particle (the effective load-carry duty 60% of Avermectin), sodium lignin sulfonate 100.0 grams, polymethylacrylic acid carboxylate graft copolymer 20.0 grams, sodium carboxymethylcellulose 5.0 grams, ammonium sulfate 100.0 grams that contain plain 5.0 grams of A Wei mattress according to prescription, supply 1000 grams with bentonite, under agravic condition, mixed 10 minutes, pulverize with airslide disintegrating mill.It is qualified to detect every technical indicator, promptly gets 5% avermectin nanometer medicine-carried system.
Embodiment 3:
Require accurately to take by weighing avermectin nanometer medicine-carried particle (the effective load-carry duty 60% of Avermectin), sodium lignin sulfonate 120.0 grams, polymethylacrylic acid carboxylate graft copolymer 25.0 grams, sodium carboxymethylcellulose 5.0 grams, ammonium sulfate 120.0 grams that contain Avermectin 10.0 grams according to prescription, supply 1000 grams with bentonite, under agravic condition, mixed 10 minutes, pulverize with airslide disintegrating mill.It is qualified to detect every technical indicator, promptly gets 10% avermectin nanometer medicine-carried system.
Embodiment 4:
Require accurately to take by weighing avermectin nanometer medicine-carried particle (the effective load-carry duty 60% of Avermectin), sodium lignin sulfonate 100.0 grams, naphthalenesulfonate formaldehyde condensation compound 20.0 grams, polymethylacrylic acid carboxylate graft copolymer 20.0 grams, sodium carboxymethylcellulose 5.0 grams, ammonium sulfate 150.0 grams that contain Avermectin 20.0 grams according to prescription, supply 1000 grams with diatomite, under agravic condition, mixed 10 minutes, pulverize with airslide disintegrating mill.It is qualified to detect every technical indicator, promptly gets 20% avermectin nanometer medicine-carried system.
Realize that best mode of the present invention is embodiment 1 and embodiment 2.
Claims (7)
1. avermectin nanometer medicine-carried system with slow-releasing and controlled-releasing action is characterized in that:
1. pesticide active ingredient is Avermectin (English general abamectin by name), and best effectively working concentration is 1～20%;
2. carrier material is a kind of nano silicon with loose structure, can effectively carry by physisorption and form avermectin nanometer medicine-carried particle after the Avermectin, and its bearing capacity to Avermectin is 10～80% of an own wt;
3. the dispersant of Shi Yonging is one or two a mixture in anion surfactant sodium lignin sulfonate, naphthalenesulfonate formaldehyde condensation compound, the polymethylacrylic acid carboxylate graft copolymer, and weight percentage is 5～20%;
4. the disintegrant of Shi Yonging is the mixture of ammonium sulfate, soluble starch, one or more filler of sodium carboxymethylcellulose, and weight percentage is 1～10%;
5. the filler of Shi Yonging is the mixture of one or more filler in white carbon, bentonite, the diatomite, and weight percentage is 10～80%;
6. medicine-carried system finally is processed into water dispersible granules (WG) formulation, and outward appearance is a cylindrical pellet, and spontaneous dispersion forms suspension to water during use.
7. the medicine-carried system hybrid mode is agravic mixing, and grinding mode is a comminution by gas stream, and the granulation mode is an extruder grain.
2. avermectin nanometer medicine-carried system according to claim 1, the weight percentage that it is characterized in that Avermectin in the medicine-carried system is 1～20%.
3. avermectin nanometer medicine-carried system according to claim 1, it is characterized in that Avermectin forms avermectin nanometer medicine-carried particle by physisorption and the nanometer silicon dioxide material with loose structure in the medicine-carried system, wherein Avermectin is 10～80% of a nanometer silicon dioxide material own wt.
4. avermectin nanometer medicine-carried system according to claim 1, it is characterized in that the dispersant that uses in the medicine-carried system is one or two a mixture in anion surfactant sodium lignin sulfonate, naphthalenesulfonate formaldehyde condensation compound, the polymethylacrylic acid carboxylate graft copolymer, weight percentage is 5～20%.
5. avermectin nanometer medicine-carried system according to claim 1 is characterized in that the disintegrant that uses in the medicine-carried system is the mixture of ammonium sulfate, soluble starch, one or more filler of sodium carboxymethylcellulose, and weight percentage is 1～10%.
6. avermectin nanometer medicine-carried system according to claim 1 is characterized in that the filler that uses in the medicine-carried system is the mixture of one or more filler in white carbon, bentonite, the diatomite, and weight percentage is 10～80%.
7. the preparation method of avermectin nanometer medicine-carried system of the present invention is, at first Avermectin and the nanometer silicon dioxide material with loose structure are formed avermectin nanometer medicine-carried particle by physisorption, accurately take by weighing by formula rate with recipe ingredients such as dispersant, disintegrant, fillers again, add in the agravic blender and fully mix, carry out comminution by gas stream then, carry out extruder grain after reaching the fineness of regulation.Final pesticide water dispersible granules (WG) formulation that forms, outward appearance is a cylindrical pellet, spontaneous dispersion forms suspension to water during use.Every after testing technical indicator is qualified, promptly gets required avermectin nanometer medicine-carried system with slow-releasing and controlled-releasing action.
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