CN101642164A - Preparation method and application of garlic essence oil nanometer-dispersion capsule as grain protective agent - Google Patents
Preparation method and application of garlic essence oil nanometer-dispersion capsule as grain protective agent Download PDFInfo
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- CN101642164A CN101642164A CN200910063465A CN200910063465A CN101642164A CN 101642164 A CN101642164 A CN 101642164A CN 200910063465 A CN200910063465 A CN 200910063465A CN 200910063465 A CN200910063465 A CN 200910063465A CN 101642164 A CN101642164 A CN 101642164A
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Abstract
The invention relates to a preparation method and application of garlic essence oil nanometer-dispersion capsule as a grain protective agent. The preparation method comprises the following steps: heating PEG 6000 to 70 DEG C to be dissolved, continuously stirring; adding garlic essence oil to the molten PEG 6000 in a conduction mode to form homogeneous oil-PEG-inclusive materials; naturally cooling, grinding, smashing and sieving by a 200-mesh sieve to obtain the garlic essence oil nanometer-dispersion capsule. The garlic essence oil nanometer-dispersion capsule is placed in a grain storage place to kill pests in stored grain. In the invention, PEG is used as a carrier, the mixed ratio of the oil to the PEG is from 1:15 to 1: 5, and the entrapment rate can reach more than 70%. High temperature is not needed in the process of garlic essence oil nanometer-dispersion capsule preparation, therefore, the volatilization of components with a low boiling point of the oil is greatly reduced, the integrity of the components of the garlic essence oil is ensured, and the duration period of the action of the garlic essence oil is prolonged. The capsule has good dispersiveness and no aggregation; the manufacture process is simple, and the production cost is low. The garlic essence oil nanometer-dispersion capsule has very wide application prospect in the agricultural technical filed of the prevention and the treatment of pests in stored grain, and the like.
Description
Technical field
The present invention relates to a kind of preparation and application of grain protectant garlic essence oil nanometer-dispersion capsule.
Background technology
Grain is important goods and the strategic materials that involve the interests of the state and the people, and has crucial meaning for economic development and social stability.During foodstuff preservation, the loss that causes because of insect pest can not be ignored.The grain storage technology of generally using can effectively be prevented and treated the harm of grain storage pest to a certain extent at present, but the drawback that they exist self also can not be ignored, strict as mechanical-physical control for infrastructure etc., need a large amount of fund inputs, serious " 3R " problem that chemical prevention caused is then very serious.Therefore " green pesticide " of seeking a kind of environment-friendly type is extremely urgent.
Garlic is the flavouring that people use always, and is without any side effects to human body, and the galic essential oil that extracts from garlic is subjected to extensive concern because of having stronger antibiotic, insecticidal activity.Yet the effumability of galic essential oil makes that the duration of its insecticidal activity is very short, thereby has limited its application aspect grain storage pest controlling.Therefore, develop a kind of galic essential oil active ingredient volatilization of slowing down, thereby can effectively prolong the effective dosage forms of galic essential oil effect duration, will have very big production application and be worth.
At present, the pesticide nano capsules preparation is one of important directions of current pesticides new formulation development.More to the preparation method of pesticide nano capsules agent both at home and abroad, commonly used have spray drying process, complex coacervation and an interfacial polymerization etc.Wherein spray drying process is most widely used, but the high temperature that uses in the spray process makes that to have volatile plants essential oil loss big; And complex coacervation and interfacial polymerization be because of complex technical process, and step is various, and relate to technical problems such as technology amplification and make that its real cost of production is higher.Therefore, seek a kind of simple, production cost is low and the Nano capsule bag carrier technology of not loss plants essential oil active ingredient is particularly important.
Summary of the invention
The objective of the invention is at above-mentioned present situation; it is good to aim to provide a kind of nanoparticulate dispersed; do not have and assemble; manufacture craft is simple, production cost is low; the bag of galic essential oil carries rate and all can reach more than 70%; good slow release is arranged, the preparation and the application of a kind of grain protectant garlic essence oil nanometer-dispersion capsule that prevention effect is good.
The implementation of the object of the invention is; a kind of preparation method of grain protectant garlic essence oil nanometer-dispersion capsule; take by weighing PEG6000 50-150g, be heated to 70 ℃ of dissolvings after, constantly stir with glass bar; and in the PEG6000 that melts, add the galic essential oil of 10ml in the mode of drainage; form uniform essential oil-polyethylene glycol fused matter, after the cooling, grind naturally; cross 200 mesh sieves, get garlic essence oil nanometer-dispersion capsule.
A kind of application of grain protectant garlic essence oil nanometer-dispersion capsule places the foodstuff preservation place to kill grain storage pest.
The present invention has following advantage:
1, with PEG is carrier, in the process of preparation essence oil nanometer-dispersion capsule, need do not use high temperature, greatly reduce the volatilization of essential oil low boiling point component, guaranteed the integrality of galic essential oil composition, prolonged the duration of galic essential oil effect;
2, the capsule of making is spherical in shape, and particle diameter is a nanoscale size, and good dispersion does not have and assembles;
3, essential oil and PEG are 1: 15-1: 5 be mixed than in the scope, the bag of galic essential oil carries rate and all can reach more than 70%.
4, manufacture craft is simple, production cost is low.
This garlic essence oil nanometer-dispersion capsule is having boundless application prospect aspect the agricultural technology fields such as control of grain storage pest.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the garlic essence oil nanometer-dispersion capsule of embodiment 1 preparation,
Fig. 2 A, B, C are the analysis of volatile components figure in garlic essence oil nanometer-dispersion capsule Bao Zaiqian, Bao Zaihou 1 day, Bao Zaihou May of embodiment 1 preparation,
Fig. 3 A1, A2 are that garlic essence oil nanometer-dispersion capsule and the galic essential oil that embodiment 1 has just prepared is applied to the insecticidal activity figure of grain storage pest after 5 days,
Fig. 4 B1, B2 are that back 1 month garlic essence oil nanometer-dispersion capsule and the galic essential oil of embodiment 1 preparation is applied to the insecticidal activity figure of grain storage pest after 5 days,
Fig. 5 C1, C2 are that back 2 months garlic essence oil nanometer-dispersion capsule and the galic essential oil of embodiment 1 preparation is applied to the insecticidal activity figure of grain storage pest after 5 days,
Fig. 6 D1, D2 are that back 3 months garlic essence oil nanometer-dispersion capsule and the galic essential oil of embodiment 1 preparation is applied to the insecticidal activity figure of grain storage pest after 5 days,
Fig. 7 E1, E2 are that back 4 months garlic essence oil nanometer-dispersion capsule and the galic essential oil of embodiment 1 preparation is applied to the insecticidal activity figure of grain storage pest after 5 days,
Fig. 8 F1, F2 are that back 5 months garlic essence oil nanometer-dispersion capsule and the galic essential oil of embodiment 1 preparation is applied to the insecticidal activity figure of grain storage pest after 5 days.
The specific embodiment
Below by embodiment and accompanying drawing in detail the present invention is described in detail.
Specific embodiments of the invention:
Example 1, take by weighing PEG6000 100g, after being heated to 70 ℃ of dissolvings, constantly stir with glass bar, and in the PEG6000 that melts, add the galic essential oil of 10ml in the mode of drainage, form uniform essential oil-polyethylene glycol fused matter, after the cooling, grind naturally, cross 200 mesh sieves, must wrap the rate of carrying and reach 80% garlic essence oil nanometer-dispersion capsule.Its nanometer transmission electron microscope figure sees Fig. 1, and as seen from the figure, the capsule that gained is made is spherical in shape, average grain diameter 101nm, and good dispersion does not have and assembles.
Example 2, with example 1, different is to take by weighing PEG6000 50g.
Example 3, with example 1, different is to take by weighing PEG6000 80g.
Example 4, with example 1, different is to take by weighing PEG6000 110g.
Example 5, with example 1, different is to take by weighing PEG6000 150g.
In order to understand fusion dispersion method preparation the main component that galic essential oil contained is had or not influence, the capsule of the applicant's use-case 1 preparation has been done the galic essential oil constituent analysis of Bao Zaiqian, Bao Zaihou 1 day, Bao Zaihou 5 months.Analytical method is, gets firm bag respectively and carries 1 day and 5 months garlic essence oil nanometer-dispersion capsule 0.1g of Bao Zaihou, is dissolved in the absolute ether of a spot of distilled water and 1ml, uses conventional extraction and extracts bag and be loaded in galic essential oil in the capsule.Utilize gas chromatography-mass spectrography technical Analysis Bao Zaiqian and bag to carry the galic essential oil composition of latter two different time sections.The condition of gas-chromatography is: HP-5MS (30m * 0.25mm * 0.25 μ m) (Agilent J﹠amp; W Scientific, USA), 60 ℃ of initial column temperatures keep 1min at 60 ℃, and the programming rate with 5 ℃/min rises to 240 ℃ again, and keeps 10min, 250 ℃ of injector temperatures, sample size 1 μ l, split ratio 1: 50 at 240 ℃.The speed of carrier gas (helium, 99.99%) is 1ml/min; The mass spectrum condition is: the EI ion gun, and electron energy 70eV, ion source temperature are 200 ℃, interface temperature is 230 ℃, sweep limits 29-400amu, electron multiplication voltage 2400V.In (The Wiley Registry of Mass Spectra Data, sixth version) every kind of compound is carried out the evaluation of molecular structure in the mass spectrometric data storehouse.Each sample repeats 3 times, and analysis result is seen Fig. 2 A, B, C.1,2 and 3 represent diallyl disulphide (diallyl disulfide) respectively among the figure, diallyl trithioether (diallyltrisulfide), allyl sulfide (diallyl sulfide).
Can find that from figure the main component that galic essential oil contained of wrapping before and after carrying does not change.The prepared garlic essence oil nanometer-dispersion capsule of presentation of results fusion dispersion method is feasible.
Carry front and back insecticidal activity and the situation of duration in order to understand the galic essential oil bag, the applicant has done the garlic essence oil nanometer-dispersion capsule of use-case 1 preparation and the comparative experiments of galic essential oil,
With the red flour beetle adult is example, adopts and mixes the grain fumigating system.Experiment divides two groups: one group is the direct application of galic essential oil, take by weighing some parts and handled (160 by the various dose galic essential oil, 320,480 and 640ppm) 100g paddy (containing 2% cracks rice) place the wide-mouth bottle of 250ml, with nylon gauze and preservative film all bottlenecks are sealed; Another group then is the application of the garlic essence oil nanometer capsule of Bao Zaihou, take by weighing some parts and handled (2000 by the various dose Nano capsule, 4000,6000 and 8000ppm, be equivalent to 160,320,480 and the essential oil amount of 640ppm unentrapped) 100g paddy (containing 2% cracks rice) place the wide-mouth bottle of 250ml, with nylon gauze and preservative film all bottlenecks are sealed.Paddy after the processing is preserved 1 day (0 month), January, February, March, April and May respectively at normal temperatures, and the paddy of handling is carried out the toxicity test analysis.
Concrete mensuration process is: 60 of red flour beetle adults dropping into hungry 24h in each is equipped with the wide-mouth bottle of processed paddy, then all bottlenecks are sealed with nylon gauze and preservative film, it is placed 28 ± 1 ℃ respectively, carry out smoked kill in the growth cabinet of 75 ± 5%r.h, check the death condition (touching the examination worm with the writing brush point, is death standard with the feeler nonresponder) of examination worm after 5 days.With the paddy that is left intact in contrast.Every processing triplicate.
Under the situation of same dose, the active result of paddy after preserving 1 day is shown in Fig. 3 A1, A2, and the insecticidal effect of the galic essential oil of unentrapped is better than the insecticidal effect of the galic essential oil of Bao Zaihou.Along with the prolongation in paddy processing time, the insecticidal effect of the galic essential oil of Bao Zaihou obviously is better than the insecticidal effect (seeing Fig. 4 B1, B2, Fig. 5 C1, C2, Fig. 6 D1, D2, Fig. 7 E1, E2) of the galic essential oil of unentrapped.
Under the dosage treatment conditions of 640ppm, preserve active result such as Fig. 8 F1, F2 after 5 months, the examination worm death rate of garlic essence oil nanometer-dispersion capsule processed group still is in more than 80%, and the examination worm death rate of the processed group of the galic essential oil of unentrapped only is 11%.
As seen from the figure, what use the preparation of fusion dispersion method is that the garlic essence oil nanometer-dispersion capsule pesticide of carrier has good slow release with PEG, has prolonged the duration of medicament, and red flour beetle is had better prevention effect.Therefore, this garlic essence oil nanometer-dispersion capsule is having boundless application prospect aspect the agricultural technology fields such as control of grain storage pest.
Claims (2)
1, a kind of preparation method of grain protectant garlic essence oil nanometer-dispersion capsule; it is characterized in that taking by weighing PEG6000 50-150g; after being heated to 70 ℃ of dissolvings; constantly stir with glass bar, and in the PEG6000 that melts, add the galic essential oil of 10ml, form uniform essential oil-polyethylene glycol fused matter in the mode of drainage; naturally after the cooling; grind, cross 200 mesh sieves, get garlic essence oil nanometer-dispersion capsule.
2, a kind of application of the grain protectant garlic essence oil nanometer-dispersion capsule by claim 1 preparation is characterized in that placing the foodstuff preservation place to kill grain storage pest.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107996701A (en) * | 2017-11-29 | 2018-05-08 | 贵州亚港气体有限公司 | A kind of preserving rice gas and its preparation method and device for formulating |
| CN113203821A (en) * | 2021-04-21 | 2021-08-03 | 中国烟草总公司郑州烟草研究院 | Application of compound, analysis protective agent and analysis method of fragrance components in plant extract |
-
2009
- 2009-08-06 CN CN200910063465A patent/CN101642164A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107996701A (en) * | 2017-11-29 | 2018-05-08 | 贵州亚港气体有限公司 | A kind of preserving rice gas and its preparation method and device for formulating |
| CN113203821A (en) * | 2021-04-21 | 2021-08-03 | 中国烟草总公司郑州烟草研究院 | Application of compound, analysis protective agent and analysis method of fragrance components in plant extract |
| CN113203821B (en) * | 2021-04-21 | 2024-05-31 | 中国烟草总公司郑州烟草研究院 | Application of compound, analysis protectant and analysis method of aroma components in plant extract |
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Open date: 20100210 |