CN105223310B - A kind of method of testing of microcapsule capsule-core release rate and device - Google Patents
A kind of method of testing of microcapsule capsule-core release rate and device Download PDFInfo
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- CN105223310B CN105223310B CN201510669844.XA CN201510669844A CN105223310B CN 105223310 B CN105223310 B CN 105223310B CN 201510669844 A CN201510669844 A CN 201510669844A CN 105223310 B CN105223310 B CN 105223310B
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Abstract
The invention discloses a kind of method of testing of microcapsule capsule-core release rate and device, belong to technical field of pesticide.In the method for testing of microcapsule capsule-core release rate of the present invention, microcapsule sample is placed in organic filter, then adds the release medium needed for a small amount of release medium, test process considerably less into organic filter；In addition, microcapsule just can will not pass through through the filter membrane in organic filter, the capsule-core being only released, the inventive method test error is very little.
Description
Technical field
The present invention relates to technical field of pesticide, particularly to a kind of method of testing of microcapsule capsule-core release rate and device.
Background technology
Microcapsule technology has application in a lot of industries at present, can effectively reduce core environment to external world using microcapsule
The reaction of factor, controls the release of core, or even change the physicochemical properties of core etc..
The slow releasing function of capsule-core material is an important characteristic of microcapsule, the slow release characteristic of detection microcapsule, permissible
Use thermogravimetry, solution release method.
Microcapsule capsule-core release rate test traditional method be：Microcapsule A is put in a large amount of release medium, stirring, fixed
When take out a certain amount of release medium, with filtering with microporous membrane, and fill into equivalent release medium, by filtrate with after solvent constant volume,
Detected, and calculated cumulative release amount, drawn release profiles.As shown in figure 1, microcapsule sample is placed in substantial amounts of release medium
In, extract a part of liquid at set intervals out, fill into the release medium of equivalent simultaneously.
The shortcoming of this method is：
1, when taking out a certain amount of release medium, inevitably take out a part of microcapsule A (being relatively large in diameter), to examination
Test result and cause error；
2, take out a certain amount of release medium, be supplemented with into after same amount of release medium, to capsule-core B（Diameter is little）Dense
Degree impact is big, so when release medium consumption is very big, error just can reduce.
Content of the invention
In order to solve in prior art that microcapsule capsule-core release rate test result error is big and test process in diluent media
The big problem of consumption, the invention provides a kind of method of testing of microcapsule capsule-core release rate and device.
The technical scheme is that：
A kind of method of testing of microcapsule capsule-core release rate, including step：
1）Prepare microcapsule release medium；
2）Microcapsule sample to be measured is placed in organic filter；
3）Microcapsule release medium is pushed into the organic filter equipped with microcapsule sample to be measured by syringe；By note
Release medium is released by emitter by organic filter, collects the material by filter membrane in organic filter, constant volume, detection, records 0min
When burst size q0；
4）After certain time t, microcapsule is pushed into the organic filter equipped with microcapsule sample to be measured by syringe and releases
Put medium, collect the release medium by filter membrane in organic filter and the capsule-core material discharging, constant volume, detection, record phase
Burst size q during t between seasonablet；
5）Repeat step 4）；
6）Cumulative release amount is calculated according to each burst size, thus calculating microcapsule capsule-core release rate.
Preferably, step 1）The compound method of described release medium is：Add a certain amount of in deionized water
Organic solvent；Described organic solvent be methanol, ethanol, dimethylbenzene, N,N-dimethylformamide, ethylene glycol, glycerol, chloroform,
Dichloromethane, mass fraction in release medium for the described organic solvent is 0-99%.
Preferably, in described organic filter, the aperture of filter membrane is 0.1-1 micron.The aperture setting of filter membrane 7 needs
Meet, microcapsule can not pass through filter membrane 7, and capsule-core material can pass through filter membrane 7.
Preferably, step 4）Middle time t is 1-20 minute, it is highly preferred that step 4）Middle time t is 8-15min.
Preferably, step 3）, step 4）In, enter microcapsule release medium 0.5-2mL to organic filter interior suction.
The method of testing equipment therefor of described microcapsule capsule-core release rate, including syringe, described syringe includes syringe
3rd, piston rod 2, piston 4 and handle 1；The front end face of described syringe 3 is provided with the first check valve installation portion 5, described first check valve
Installation portion 5 is connected with the entrance of the first check valve 6, and the exit of described first check valve 6 is provided with organic filter 8, described organic
In filter 8, the aperture of filter membrane 7 is 0.1-1 micron；The side wall of described syringe 3 is provided with the second check valve installation portion 9, and described second is single
Connect to valve installation portion 9 with the entrance of the second check valve 12, the exit of described second check valve 12 is provided with needle holder 10, described
Equipped with syringe needle 11 in needle holder 10.
Wherein, the first check valve 6 and the second check valve 12 are reverse check valve, and the first check valve 6 only allows material by pin
It flow to outside syringe in cylinder；Second check valve 12 only allows material to be entered inside syringe by outside syringe.In addition, in syringe 3 side wall
Second check valve installation portion 9 is set, and the second check valve installation portion 9 needs the front end face near syringe 3, and in general second is unidirectional
The center of valve installation portion 9 is 2-5mm with the vertical dimension of syringe 3 front end face；And, piston 4 is pushed into the second check valve installation portion 9
When, piston will not enter the second check valve installation portion 9, but continues to move ahead through the second check valve installation portion 9.
Preferably, described syringe 3 outer wall is provided with graduation mark 13.
Preferably, described second check valve installation portion 9 is provided with a grade net with syringe 3 joint.Arranging shelves net is exactly
In order to prevent piston 4 from entering the second check valve installation portion 9, and bottom can not be shifted onto, or using inconvenience.
Preferably, the space of described second check valve installation portion 9 and syringe 3 joint is less than the thickness of piston 4.
Joint space is little, and piston 4 can not enter, and this is another kind of scheme preventing piston 4 from entering the second check valve installation portion 9.
Beneficial effects of the present invention are：
Microcapsule sample is placed in organic filter the present invention, then adds a small amount of release medium into organic filter,
Release medium needed for test process is considerably less；In addition, microcapsule only will not be released through the filter membrane in organic filter
The capsule-core coming just can pass through, and the inventive method test error is very little.
Brief description
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
Have technology description in required use accompanying drawing be briefly described it should be apparent that, drawings in the following description be only this
Some embodiments of invention, for those of ordinary skill in the art, without having to pay creative labor, also may be used
So that other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the test philosophy schematic diagram of prior art microcapsule capsule-core release rate；
Fig. 2 is the test philosophy schematic diagram of microcapsule capsule-core release rate of the present invention；
Fig. 3 is the graph of a relation of microcapsule capsule-core release rate and time；
Fig. 4 is the structural representation of the method for testing equipment therefor of microcapsule capsule-core release rate.
Specific embodiment
Embodiment 1
As shown in figure 4, the method for testing equipment therefor of microcapsule capsule-core release rate, including syringe, syringe includes pin
Cylinder 3, piston rod 2, piston 4 and handle 1, syringe 3 outer wall is provided with graduation mark 13.
The front end face of syringe 3 is provided with the first check valve installation portion 5, and the first check valve installation portion 5 is entered with the first check valve 6
Mouth connects, and the exit of the first check valve 6 is provided with organic filter 8, and in organic filter 8, the aperture of filter membrane 7 is 0.1-1 micron.Filter
The aperture setting of film 7 needs to meet, and microcapsule can not pass through filter membrane 7, and capsule-core material can pass through filter membrane 7.
The side wall of syringe 3 is provided with the second check valve installation portion 9, and the second check valve installation portion 9 is entered with the second check valve 12
Mouth connects, and the exit of the second check valve 12 is provided with needle holder 10, equipped with syringe needle 11 in needle holder 10.
Wherein, the first check valve 6 and the second check valve 12 are reverse check valve, and the first check valve 6 only allows material by pin
It flow to outside syringe in cylinder；Second check valve 12 only allows material to be entered inside syringe by outside syringe.
In addition, arranging the second check valve installation portion 9 in syringe 3 side wall, the second check valve installation portion 9 needs near syringe 3
Front end face, in general the vertical dimension of the center of the second check valve installation portion 9 and syringe 3 front end face is 2-5mm；And,
When piston 4 is pushed into the second check valve installation portion 9, piston will not enter the second check valve installation portion 9, but through the second check valve
Installation portion 9 continues to move ahead.Preferably, the second check valve installation portion 9 is provided with a grade net with syringe 3 joint.Setting shelves net
Exactly in order to prevent piston 4 from entering the second check valve installation portion 9, and bottom can not be shifted onto, or using inconvenience.As another kind of preferred
Scheme, the space of the second check valve installation portion 9 and syringe 3 joint is less than the thickness of piston 4.Joint space is little, and piston 4 is not
Can enter, this is another kind of scheme preventing piston 4 from entering the second check valve installation portion 9.
A kind of method of testing of microcapsule capsule-core release rate, including step：
1）Prepare microcapsule release medium：Take 30g methanol, mix homogeneously with 70g deionized water；
2）Weigh the chlorpyrifos microcapsule sample that 0.1002g active constituent content is 30%, and by this chlorpyrifos microcapsule sample
Product are placed in organic filter 8, and in this organic filter 8, the aperture of filter membrane 7 is 0.22 micron；
3）Organic filter 8 is installed on the first check valve 6；Syringe needle 11 is inserted in the aqueous solution of methanol, extracts 1mL and release
Put medium, and push to organic filter 8, simultaneously in the port of export reception filtrate of organic filter 8, be settled to 25mL, examined
Survey, burst size q during record 0min0；
4）After 20min, again syringe needle 11 is inserted in the aqueous solution of methanol, extract 1mL release medium, and push to having
Machine filter head 8, the liquid in organic filter 8 is released, and receives filtrate in the port of export of organic filter 8, is settled to 25mL, is examined
Survey, burst size q during record 20min20.
5）Repeat step 4）, and record burst size q of each time respectively40、q60、q80……qn0；
6）Cumulative release amount is calculated according to each burst size, thus calculating microcapsule capsule-core release rate.Draw microcapsule
Capsule-core release rate and the curve chart of time.
As shown in Fig. 2 microcapsule sample is placed in organic filter the present invention, release is then added to be situated between into organic filter
Matter, the release medium needed for test process is considerably less；And, microcapsule A only will not be released through the filter membrane in organic filter
The capsule-core B releasing just can pass through, and the inventive method test error is very little.
Wherein,
.
In chlopyrifos microcapsule suspending agent, the assay method of capsule-core material total content is：30% chlorpyrifos microcapsule is suspended
Agent, 0.1002g sample, transfer in 100mL volumetric flask with methanol, ultrasonic cell disruption instrument breaks capsule, again with methanol is settled to
100mL, the total content of high effective liquid chromatography for measuring chlopyrifos microcapsule suspending agent.Prepare mobile phase methanol：Water=90:10.
From the figure 3, it may be seen that the burst effect at release initial stage is obvious.With the carrying out of release process, the rate of release of microcapsule by
Decrescence slow, during 14h, the cumulative release amount of microcapsule is respectively 91.22%.The Cumulative release profile of microcapsule carries out kinetic model plan
Close its accumulative release rule and all meet first _ order kinetics equation：.
Claims (5)
1. a kind of method of testing of microcapsule capsule-core release rate is it is characterised in that include step： 1）Prepare microcapsule release to be situated between
Matter； 2）Microcapsule sample to be measured is placed in organic filter； 3）By syringe to organic equipped with microcapsule sample to be measured
Microcapsule release medium is pushed in filter；By syringe, release medium is released by organic filter, collect and pass through organic filter
The material of middle filter membrane, constant volume, detection, burst size q0 during record 0min； 4）After certain time t, by syringe to equipped with treating
Push microcapsule release medium in organic filter of micrometer capsule sample, collect release medium by filter membrane in organic filter and
The capsule-core material discharging, constant volume, detection, record burst size qt during corresponding time t； 5）Repeat step 4）； 6）According to
Each time burst size calculates cumulative release amount, thus calculating microcapsule capsule-core release rate.
2. as described in claim 1 method of testing of microcapsule capsule-core release rate it is characterised in that step 1）Described release is situated between
The compound method of matter is：Add a certain amount of organic solvent in deionized water；Described organic solvent is methanol, ethanol, diformazan
Benzene, N, N- dimethylformamide, ethylene glycol, glycerol, chloroform, dichloromethane, matter in release medium for the described organic solvent
Amount fraction is 0-99%.
3. as described in claim 1 microcapsule capsule-core release rate method of testing it is characterised in that：Filter in described organic filter
The aperture of film is 0.1-1 micron.
4. microcapsule capsule-core release rate as claimed in claim 2 method of testing it is characterised in that：Step 4）Middle time t is 1-
20min.
5. as described in any one of claim 1-4 microcapsule capsule-core release rate method of testing it is characterised in that：Step 3）, step
Rapid 4）In, enter microcapsule release medium 0.5-2mL to organic filter interior suction.
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| CN201510669844.XA CN105223310B (en) | 2015-10-16 | 2015-10-16 | A kind of method of testing of microcapsule capsule-core release rate and device |
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| CN201510669844.XA CN105223310B (en) | 2015-10-16 | 2015-10-16 | A kind of method of testing of microcapsule capsule-core release rate and device |
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| CN105223310B true CN105223310B (en) | 2017-03-01 |
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| CN106198805A (en) * | 2016-07-12 | 2016-12-07 | 中山大学惠州研究院 | A kind of detection method of spices and essence Controlled-Release Capability of Microcapsules |
| CN113358777B (en) * | 2021-06-02 | 2022-09-16 | 江苏徐淮地区淮阴农业科学研究所 | Detection device box and detection method for release rate of microcapsule active ingredients |
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| US20060154378A1 (en) * | 2005-01-13 | 2006-07-13 | Yabin Lei | Method for measuring the leaching of encapsulated material into application media |
| KR100816065B1 (en) * | 2006-11-27 | 2008-03-24 | 동국제약 주식회사 | Preparation method of sustained-release microcapsules having good initial burst inhibiting property and the microcapsules thereby |
| CN101721677B (en) * | 2008-10-10 | 2012-01-25 | 北京博恩特药业有限公司 | Thymopentin oral microsphere preparation and preparation method thereof |
| CN102375047B (en) * | 2011-07-15 | 2014-10-08 | 西南交通大学 | Method for determining release of chewing medicament and special chewing device thereof |
| CN102998202A (en) * | 2011-09-14 | 2013-03-27 | 倪蕊 | Method for determining release rate of liquid microcapsule gel breaker |
| CN102657156B (en) * | 2012-04-13 | 2013-08-28 | 西南林业大学 | Preparation of beta-cyclodextrin sustained-release microcapsule of forestry insect repellant (E)-2-hexenal and determination method |
| CN103592411B (en) * | 2013-09-05 | 2016-06-22 | 深圳大学 | A kind of method of testing of capsule core release amount of concrete chemical self-repair microcapsule |
| CN104535688B (en) * | 2014-12-31 | 2016-07-13 | 辰欣药业股份有限公司 | A kind of assay method of Sustained Release Ambroxol Hydrochloride Capsules release |
| CN205027718U (en) * | 2015-10-16 | 2016-02-10 | 山东农业大学 | Used device of microcapsule capsule -core release rate test |
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