CN101743991B - SF-embedded termite drug and preparation method and application thereof - Google Patents
SF-embedded termite drug and preparation method and application thereof Download PDFInfo
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- CN101743991B CN101743991B CN 200910214113 CN200910214113A CN101743991B CN 101743991 B CN101743991 B CN 101743991B CN 200910214113 CN200910214113 CN 200910214113 CN 200910214113 A CN200910214113 A CN 200910214113A CN 101743991 B CN101743991 B CN 101743991B
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Abstract
The invention discloses an F-embedded termite drug and a eparation method and application thereof. The preparation method comprises the following steps: (1) slk fibroin and N-amber Asian amide in 1:100 mass ratio are dissolved in 1-fluorine-2,4-dinitrobenzene and PBS, and are mixed and react in ice bath, to form optical-activity silk fibroin solution; (2) the optical-activity silk fibroin solution is dripped on the surface of clean material, a termite drug is added in, and another layer of optical-activity silk fibroin solution is paved on to be cooled, dried, embedded, radiated by ultraviolet light for 15 to 20min, so that the embedded drug is grafted to the material, and the SF-embedded termite drug is prepared. The SF-embedded termite drug prepared by the method of the invention has the effect of long-time effect and releasing, improves the toxic effect to the termite, and reduces the pollution caused by the termite drug to the environment.
Description
Technical field
The present invention relates to the preparation field of white-ant drug, be specifically related to white-ant drug of a kind of fibroin albumen embedding and its preparation method and application.
Background technology
Cryptotermes Insecta Pterigota Isoptera mainly contains Mastotermitidae, Hodotermitidae, Kalotermitidae, Rhinotermitidae, tooth Termitidae and Termitidae etc.Termite is destructive great worldwide insect, and distribution is all arranged all over the world, and its harm has almost related to the every field of national economy, mainly concentrates on building construction, reservoir dam, mountain forest orchard, communication apparatus and cultural relics and historic sites etc.According to estimates, the economic loss that causes of China termite is annual about 20 ~ 2,500,000,000 yuan.After nation-building portion builds a house [1993] No. 166 literary compositions " about conscientiously carrying out the notice of newly constructed house termite prevention work ", in China ant evil zone, carried out the preventing and controlling that prevent the building termite especially household to be had the coptotermes formosanus of significant damage gradually, coptotermes formosanus belongs to Insecta-Pterigota-Isoptera-Termitidae-coptotermes formosanus genus-coptotermes formosanus kind.Its harm characteristics are that building is amphibious, can build a nest underground, can nest in timber again, to the harm maximum of building construction.
The subject matter of termite control work at present is, mainly be to adopt hypertoxic gas to carry out the building foundation to handle during building prevention ant evil is implemented, or spraying ground etc. with organochlorine Niran and arsenic etc., this causes great pollution for environment especially groundwater environment.Therefore, in order to protect environment and people ' s health, low research and development of polluting the environmental protection white-ant drug there is very important meaning.
The termite prevention mainly contains chemical barrier method, physical barriers method, trapping method and insect comprehensive regulation method.Chemoprophylaxis forms chemical barrier with medicine at ground, and its short-term effect of drugs is good, but the long-term back drug wastage that uses lowers drug effect, and causes the pollution of surrounding enviroment; The physical barriers method is to adopt the big stainless steel of aperture density or gravel as physical barriers, can keep long-term control efficiency, but the cost height, it is excessive easily to cause the wasting of resources and Financial cost to drop into; The trapping method is to use food or fragrance and chemical agent to make poison bait, and sets up the poison bait observation station, and drug dose can rationally be controlled, and environmental pollution is little, and control efficiency is lasting, but the manpower and financial resources cost has high input; The insect comprehensive regulation is according to the relation of conforming between pest and the environment, the control action of performance natural cause, take multiple requisite measure, pest is controlled under the economic loss level, can reach maximum economy, society and ecological benefits, but it is too high that needed science and technology and warning monitoring system require, and do not meet with present social development level.
Tradition termite medicine mainly contains organochlorine medicine, arsenic, mirex and Biphenthrin etc., mainly is divided into contagious infection and causes the dead and deadly two big classes of food poisoning of neurotoxic.Because the difference of various pharmaceutical chemistry structures, decomposition rate is also different under its nature, and it is big to pollute cycle long-range degree for a long time simultaneously as arsenic steady chemical structure, drug effect.The Biphenthrin chemical constitution is active relatively, and short pollution of half life period is light but drug effect is not lasting.
The pollution problem of let us living environment aggravation when the termite medicine uses, even injured we self health, this using method with traditional white-ant drug be unable to do without.The termite medicine is mainly used in real estate and the orchard planting, or liquid sprays or the mode of the buried soil of solid is isolated or eliminate termite.So just air and soil environment have been caused serious pollution.The rainwater effect enlarges the medicine groundwater environment that induces one to pollute and also causes drug effect to run off in addition, also is that white-ant drug can not be brought into play one of reason of effect for a long time.
In recent years, fibroin albumen is widely used in fields such as biology sensor, biomedical material and preparation fibroin membrane because have nontoxic, non-stimulated, as to have a good physics and chemical property and biocompatibility natural macromolecular material as a kind of by people.Wherein fibroin albumen has also attracted many scientists to pay attention to as the research of drug controlled release material (being pharmaceutical carrier).Pharmaceutical carrier rises gradually with the development of biomaterial science, clinical medicine and pharmacology.Its substantive characteristics is that the carrying person as medicine makes medicine bring into play effectiveness better.The position that the advantage of the various pharmaceutical carriers that have been applied at present is medicine is discharged, speed, mode etc. have selectivity and controllability.Fibroin albumen just has the application report of success as far back as the eighties of last century the eighties in the research aspect immobilized enzyme and the antibody as the fixation support material.General simple investment and the covalent cross-linking method of adopting of fibroin albumen immobilized enzyme, utilize these methods successively to develop fibroin immobilized glucoamylase, fibroin immobilized catalase, fibroin immobilization pectase, fibroin immobilization-amylase etc., enzyme after fixing is stronger to the resistivity of poor environment, have long operation half life period, optimal reaction pH and optimal reactive temperature scope wider, the vigor of enzyme also increases.Use fibroin albumen embedding connection 5 FU 5 fluorouracil in the research, medicine is fixed in certain material membrane, can also regulate release rate of drugs according to the aperture of made film.
Begin till now the beginning of the nineties from eighties of last century, the researcher has had very great development to the research of photochemical fixation method both at home and abroad.The photofixation method be be fixed on the bioabsorbable polymer material surface by grafting material (as polypeptide, enzyme, growth factor, protein etc.), prepare have various activity, various uses biomaterial.Studies show that the hematopoietin after the photofixation still has cell stimulating activity, and the specific ionization state is remarkable.The time of photo-immobilization epithelial cell growth factor specific ionization epithelial cell growth factor transmission signal is longer.The immobilization phycocyanin brings up to 55% to 7402 cell inhibitory rates by not immobilized 6%.Research also shows, is total to photo-immobilization
With
When 20ng/well dosage, the activity that suppresses the growth of HeLa cell reaches 82% (48h), and has long-effect active, and 120h suppresses activity can be up to 92%.This method can reduce greatly the purpose coating reagent polymer surface produce unordered crosslinked, make the surface ratio of modification with other surface coating method gained surfaces more significant activity be arranged, and having characteristics such as the unexistent slowly-releasing of common drug, long-acting advantage, is one of developing direction of newtype drug.
Summary of the invention
The objective of the invention is to according to the deficiencies in the prior art, a kind of white-ant drug of fibroin albumen embedding is provided.
Another object of the present invention is to provide the preparation method of the white-ant drug of above-mentioned fibroin albumen embedding.
A further object of the invention provides the application of said medicine.
Above-mentioned purpose of the present invention is achieved by the following technical programs:
A kind of white-ant drug of fibroin albumen embedding comprises following component: fibroin albumen, and the inferior acid amides of N-amber and Biphenthrin, the mol ratio of three components is 5: 500: 1.。
The preparation method of the white-ant drug of fibroin albumen embedding of the present invention comprises the steps:
(1) be that 1: 50 ~ 1: 500 the inferior acid amides of fibroin albumen and N-amber mixes with mol ratio, be dissolved in 1-fluoro-2, among 4-dinitro benzene and the PBS, ice bath hybrid reaction, formation photolytic activity silk fibroin protein solution;
(2) drip the photolytic activity silk fibroin protein solution at clean material surface, add Biphenthrin, repave one deck photolytic activity silk fibroin protein solution, make five times of excessive embedding Biphenthrins of mole of fibroin albumen, after-4 ℃ of freeze drying embeddings, UV-irradiation 15～20min grafts on the material, namely the medicine after the embedding.
In the above-mentioned preparation process (1), owing on the fibroin albumen a large amount of carboxyls, amino and hydroxyl are arranged, have the amino generation condensation reaction of hydrogen on the carboxyl on the inferior acid amides of N-amber and the albumen, have active fibroin albumen so can form.This process is preferably under the lucifuge condition carries out, to guarantee the activity of the inferior acid amides of N-amber.
In the above-mentioned preparation process (2), described material is preferably timber or plastics.Fibroin albumen is the big molecule of network structure that contains a large amount of amino, carboxyl and hydroxyl; therefore between the functional group condensation reaction takes place very easily; behind UV-irradiation; azido on the photolytic activity fibroin albumen produces very active nomadic nitrogen atom; it can grab in timber or the plastics on the carbon atom with hydrogen; thereby form the N-C key, the medicine after the embedding is grafted on timber or the plastics.
In the above-mentioned preparation process (2), when selecting Biphenthrin as white-ant drug for use, kill the minimum standard of termite according to Biphenthrin, the amount that adds Biphenthrin is 1 μ g/cm
2-7.5 μ g/cm
2
Compared with prior art, the present invention has following beneficial effect:
(1) after the present invention adopts embedding and photochemical fixation method to modify the termite medicine, makes the termite medical instrument be equipped with the good characteristic of nano-grade medicine, improved the toxic action to termite;
(2) white-ant drug of fibroin albumen embedding of the present invention has been regulated release rate of drugs owing to be fixed in the fibroin albumen, has increased the drug effect of medicine;
(3) drug effect of the white-ant drug of fibroin albumen embedding of the present invention when low dosage obviously strengthens, and the poisoning termite is satisfactory for result.
Description of drawings
Fig. 1 is fibroin albumen embedding Biphenthrin white-ant drug schematic diagram;
Fig. 2 is the infrared spectrogram of the inferior acid amides of N-amber, fibroin albumen and photolytic activity fibroin albumen;
Fig. 3 is electron-microscope scanning figure (60 *) as a result, and wherein, a is the electron-microscope scanning figure as a result on wood chip surface, and b is the fibroin albumen electron-microscope scanning figure as a result that is grafted on the wooden unit, and c is the electron-microscope scanning figure as a result of the fibroin albumen of embedding Biphenthrin on the wooden unit;
Fig. 4 is the fibroin albumen embedding medicinal drug effect comparison diagram that the variable concentrations Biphenthrin grafts on wooden unit;
Fig. 5 is the drug effect comparison diagram of the free drug of variable concentrations Biphenthrin;
Fig. 6 is that 1.25 μ g Biphenthrins graft on the fibroin albumen embedding medicinal of wooden unit and the drug effect comparison diagram of free drug;
Fig. 7 is that 2.5 μ g Biphenthrins graft on the fibroin albumen embedding medicinal of wooden unit and the drug effect comparison diagram of free drug;
Fig. 8 is that 7.5 μ g Biphenthrins graft on the fibroin albumen embedding medicinal of wooden unit and the drug effect comparison diagram of free drug.
Embodiment
Further explain the present invention below in conjunction with embodiment, but embodiment does not do any type of restriction to the present invention.
Get mass ratio and be 1: 100 fibroin albumen and the inferior acid amides of N-amber, two kinds of raw material reagent are added 1-fluoro-2, in 4-dinitro benzene and the PBS solution, be made into mixed solution, after the concussion evenly, under condition of ice bath, place stirring reaction on the magnetic stirring apparatus, form the photolytic activity fibroin albumen.Prepare clean wooden unit, tiling splashes into the photolytic activity silk fibroin protein solution, add white-ant drug, layer overlay photolytic activity silk fibroin protein solution in the above places freeze drying in-4 ℃ of refrigerators again, after the drying material is carried out UV-irradiation 15min, the medicine after the embedding is grafted on the wooden unit.
The monitoring of embodiment 2 photolytic activity fibroin albumen synthetic effects
In order to determine that the inferior acid amides of fibroin albumen and N-amber reacts and produces the fibroin albumen with active group, so use infrared spectrum detection product.The structure of infrared spectrum and molecule is closely related, the position of different functional groups and structure are all different to the absorption value of infrared spectrum in the molecule, utilize method of infrared spectrophotometry can measure the bond distance of molecule, bond angle, and infer the spatial configuration of molecule thus, be a kind of effective means that research characterizes molecular structure.Fibroin albumen generates the photolytic activity fibroin albumen after reacting, its molecular radical will inevitably change, and the checking fibroin albumen is synthetic from infrared spectrogram.Owing to contain a large amount of amino (peak value: about 3600) and carboxyl in the fibroin albumen, mainly there is azido (peak value 2110 ~ 2139) in the inferior acid amides of N-amber, be with the amino polymerization reaction take place of hydrogen under certain condition in the inferior acid amides of N-amber in carboxyl on the phenyl ring and the fibroin albumen, form the N-C key.
Synthetic photolytic activity fibroin albumen is owing to be with N
3Therefore 2122 INFRARED ABSORPTION peak value appears in group in infrared spectrogram.In addition, in correlative study, show, formed the N-C key and can make original material at 3500cm
-1The infrared spectrum peak narrow down, the last figure of contrast is the amino INFRARED ABSORPTION peak value relative narrower that also becomes in the fibroin albumen as can be seen, therefore can prove fibroin albumen success react with the inferior acid amides of N-amber and generate photolytic activity fibroin albumen (Fig. 2).
Material surface structural analysis after the embodiment 3 grafting newtype drugs
Use the material surface structure after electron microscope scanning is observed the grafting newtype drug, distribution and the size of medicine after the embedding effect of analysis fibroin albumen, the embedding.Electron microscope is according to electron-optical concept, replaces light beam and optical lens with electron beam and electron lens, makes the instrument of fine structure imaging under very high multiplication factor of material.The electron beam of sweep electron microscope does not pass sample, only inspires secondary electron in sample surfaces scanning, therefore utilizes the resultant graphical analysis of a scanning electron-microscopic observation surface texture at this material.From the electron-microscope scanning result, can prove, being immobilized onto material surface behind the fibroin protein film embedding medicinal presents with sheet, the particle size of Biphenthrin is about 100 ~ 200nm in the wooden unit after embedding and immobilization, and be evenly distributed, i.e. the novel embedded immobilization medicine granule medicament that is nano-scale.Studies show that in a large number nano-grade medicine has multiple good characteristic, but as good stable, little to gastrointestinal irritation, toxic and side effect is little, drug utilization degree height target administration, (Fig. 3) such as slow releasing functions arranged.
The experiment made on the living of embodiment 4 immobilization embedded medicines
Under equivalent environment and condition, cultivate termite, the wooden unit of the wooden unit of the wooden unit of the no medicine of design, the free drug of variable concentrations gradient and the immobilization medicine of respective concentration gradient, and use it to feed termite, the lethality of termite respectively organized every day in record, by utilize the statistical analysis medicine lethality rate come Primary Study that visual test and medicinal application are carried out in immobilization pharmaceutical fixed embedding effect.
Biphenthrin has characteristics such as half life period weak point, strong drug action, is present active drug as termite control.Because its half life period is shorter, use Biphenthrin can avoid the long-term pollution accumulation effect of using the back environment, but factors such as rain drop erosion simultaneously can allow drug effect in the surrounding enviroment diffuse pollution, and effective dose of the original unabiding Biphenthrin of drug effect is reduced rapidly.Chemical stability in the time of if can improving Biphenthrin and use, and as far as possible avoid the interference of extraneous factor, just can be on the basis of environmental protection better control termites for a long time.
The living environment of our the normal coptotermes formosanus of simple analog in experiment, because the cloudy happiness of termite happiness is wet, use the culture dish after sterilization of 9cm size in the time of simulated environment, and at the fine sand that was paved with bottom it behind 50 mesh sieve plates sieve, quantitatively drip the pure water of 200-300 μ g every day in fine sand, as the growing space of one group of 30 termite.
The Biphenthrin white-ant drug is used in experiment made on the living, observe the drug effect contrast of its free state and embedding stationary state, containing of following variable concentrations of novel embedding white-ant drug, free drug are set and do not have 3 groups of materials nursings of medicine termite, observe its animation and survival rate.
Fig. 4 is the novel embedding medicinal drug effect comparison diagram that the variable concentrations Biphenthrin grafts on wood chip, and Fig. 5 is the drug effect comparison diagram of the free drug of variable concentrations Biphenthrin.Obviously, the drug effect of free drug is to raise and strengthen along with drug concentrations, is near-linear dependency, namely in actual use drug dose more the multiple-effect fruit can be more obvious, but so not only cause the wasting of resources also can pollute environment easily.
Embedding and fixedly behind the Biphenthrin, significant change has taken place drug effect: 1) drug effect does not always present linear change along with the change of drug concentration; 2) in the concentration range of this experimental selection, the novel embedded immobilization medicine effect of low concentration is stronger.
There are some researches show that the peak value peak of drug effect can appear in the immobilization medicine when a certain optimum concentration.Though this optimum concentration can appear in the different concentration ranges in different immobilization medicines, but low concentration immobilization medicine often close to this just when, the drug effect of 1.25 μ g consumptions of immobilization Biphenthrin is apparently higher than the medicine of other two high concentration consumptions in this experiment.
Free medicine shows with the effect of drugs of novel immobilization medicine under each concentration, and below the general contrast these both more clearly.Obviously, 1) high concentration medicine has slow release effect after embedding, concentration medicine descends, it is medicine poisoning power main reasons for decrease, 2) in the concentration range of selecting, 1.25 all comparatively near optimum dose scope (Fig. 6 ~ 8), therefore, the drug effect of immobilization medicine is higher than the effect of free drug for μ g consumption and 2.5 μ g consumptions.
Claims (4)
1. the white-ant drug of a fibroin albumen embedding is characterized in that described medicine comprises following component: fibroin albumen,
NThe inferior acid amides of-amber and Biphenthrin, described fibroin albumen and
NThe mass ratio of the inferior acid amides of-amber is 1:100;
Described white-ant drug is the white-ant drug that is got by the method preparation that comprises the steps:
(1) with mass ratio be 1:100 fibroin albumen and
NThe inferior acid amides of-amber mixes, and is dissolved in 1-fluoro-2, and among 4-dinitro benzene and the PBS, the ice bath hybrid reaction forms the photolytic activity silk fibroin protein solution;
(2) drip the photolytic activity silk fibroin protein solution at clean material surface, add Biphenthrin, repave one deck photolytic activity silk fibroin protein solution, after the freeze drying embedding, UV-irradiation 15 ~ 20min grafts on the material, namely the medicine after the embedding.
2. according to the white-ant drug of the described fibroin albumen embedding of claim 1, it is characterized in that step (1) is to carry out under the lucifuge condition.
3. according to the white-ant drug of the described fibroin albumen embedding of claim 2, it is characterized in that in the step (2), described material is timber or plastics.
4. according to the white-ant drug of the described fibroin albumen embedding of claim 2, it is characterized in that the amount of step (2) adding Biphenthrin is 1 μ g/cm
2-7.5 μ g/cm
2
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| WO2004050316A1 (en) * | 2002-12-05 | 2004-06-17 | Osmose (Australia) Pty Ltd | Surface treatment for wood and wood products |
| CN101244277A (en) * | 2008-02-14 | 2008-08-20 | 苏州大学 | Medicine carrying fibroin microsphere and preparation thereof |
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| CN101244277A (en) * | 2008-02-14 | 2008-08-20 | 苏州大学 | Medicine carrying fibroin microsphere and preparation thereof |
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