CN110082333A - A kind of preparation method of Cucurbituril [7] Studies of Fluorescent Film Sensors - Google Patents
A kind of preparation method of Cucurbituril [7] Studies of Fluorescent Film Sensors Download PDFInfo
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- CN110082333A CN110082333A CN201910443081.5A CN201910443081A CN110082333A CN 110082333 A CN110082333 A CN 110082333A CN 201910443081 A CN201910443081 A CN 201910443081A CN 110082333 A CN110082333 A CN 110082333A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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Abstract
The invention discloses a kind of preparation methods of Cucurbituril [7] Studies of Fluorescent Film Sensors, the present invention is mainly the light polymerization method utilized in chemical method, the Cucurbituril [7] of derivatization and methyl methacrylate monomer are bonded to methacrylic acid 3-(trimethoxy silane by polymerization) propyl ester silanised quartz glass sheet surface, Cucurbituril [7] Studies of Fluorescent Film Sensors is made.Including 3 steps, quartz glass plate is put into Piranha etching liquid removes all organic matters first, placed into NaOH concentrated solution and impregnate, the acid for thoroughly neutralizing surface, allows the hydroxyl on surface to be completely exposed, and then uses distilled water flushing surface, until clean, then after by its silanization；Then Cucurbituril [7] film solution is prepared, finally uniformly contacts quartz glass plate with solution, and ultraviolet lighting carries out Photoinitiated reactions, up to Cucurbituril [7] Studies of Fluorescent Film Sensors after then cleaning.The present invention have many advantages, such as performance it is stable, it is reusable, do not pollute system to be measured, be simplicity, quick.
Description
Technical field
The present invention relates to chemical sensor field, specially a kind of preparation method of Cucurbituril [7] Studies of Fluorescent Film Sensors.
Background technique
Fluorescent optical sensor has many advantages, such as that highly selective, highly sensitive, can to acquire signal abundant and easy to use, in recent years
It is developed rapidly, is used widely in the different fields such as trace and micro-analysis, biomolecule identification.Fluorescent optical sensor
It is broadly divided into two classes, it may be assumed that homogeneous fluorescent sensor and Studies of Fluorescent Film Sensors.By homogeneous fluorescent sensor intrinsic be easy to
The disadvantages of polluting system to be measured, can only be disposable, reagent consumption is big, is restricted its use.Film fluorescence sensing
Device have many advantages, such as stability it is high, it is reusable, do not pollute system to be measured, be easy to device, conduct a research and constituted to it
The important content of current monolayer chemical research, also becomes a most active branch.
However, up to the present, preparing closely related Sensing elements in stromal surface with Studies of Fluorescent Film Sensors design
The surface chemistries Study on Problems such as distribution, existence and its state change in sensing process it is difficult because characterizing due to be difficult to depth
Enter to carry out, relevant theoretical modeling is also very weak, most to be still in the behavioral study stage, cause real device, can
It is few in number with the Studies of Fluorescent Film Sensors for being put to practical application.Homogeneous fluorescent chemical sensor principle is borrowed, design prepares thin
Film fluorescent optical sensor is the effective way that fluorescent optical sensor is pushed to practical application or expands application.
Cucurbituril [7] itself has good recognition performance, calabash to morphinane alkaloids such as jamaicin, palmatine, coptisines
The addition of reed urea [7] significantly increases the fluorescence of the morphinane alkaloids such as non-blooming jamaicin, palmatine, existing with Cucurbituril
[7] fluorimetry of the morphinane alkaloids such as homogeneous fluorescent sensor measurement jamaicin, palmatine, is mainly disadvantageous in that
Measurement requires that Cucurbituril [7] are added every time, causes system to be measured to pollute, cannot reuse.Therefore need to solve these medicines
Sensitive, accurate, efficient, the quick measurement of object, while the problem of do not pollute system to be measured.
Summary of the invention
The present invention in order to solve the morphinane alkaloids such as jamaicin, palmatine, coptisine it is quick measurement and do not pollute to
The problem of survey system, provides a kind of preparation method of Cucurbituril [7] Studies of Fluorescent Film Sensors.
The present invention is achieved by the following technical solution: a kind of preparation side of Cucurbituril [7] Studies of Fluorescent Film Sensors
Method includes the following steps:
(1) quartz glass plate is impregnated to 48 ~ 96 h in Piranha etching liquid, removes the organic matter on surface；Place into 1.5-2.5
mol·L–1NaOH solution in impregnate 6 ~ 8 h, thoroughly neutralize surface acid, allow the hydroxyl on quartz glass plate surface to be completely exposed；
Quartz glass plate is then taken out, with distilled water flushing surface, until clean；Quartz glass plate is put into 1 ~ 1.5 molL again–1
Methacrylic acid 3-(trimethoxy silane) in propyl ester silane finish aqueous solution, impregnate 11 ~ 14 h；
(2) a certain amount of allyloxy Cucurbituril [7] is added in n,N-Dimethylformamide solution, is then added a certain amount of
In the n,N-Dimethylformamide solution of methyl methacrylate monomer, a certain amount of diphenyl ketone photo initiator and peace are added
Fragrant ether photosensitizer is ceased, 15 min of ultrasound are mixed them thoroughly；
(3) well-mixed solution drop is gently put into the quartz glass plate of first step silanization, gently on polyfluortetraethylene plate
It is light to squeeze, keep the solution layer below sheet glass uniform, there cannot be bubble；It is carried out with the ultraviolet lighting of 254 nm light-initiated anti-
It answers, after reacting 1.5 ~ 2.5 h, quartz glass plate is sequentially placed into water, 15 ~ 20 min of ultrasound in ethyl alcohol, uses secondary distilled water
It rinses, forms one layer of uniform film on quartz glass plate surface, obtain Cucurbituril [7] Studies of Fluorescent Film Sensors.
The present invention is mainly the light polymerization method utilized in chemical method, by the Cucurbituril [7] and methacrylic acid of derivatization
Methylmethacrylate monomer is bonded to methacrylic acid 3-(trimethoxy silane by polymerization) propyl ester silanised quartz glass sheet surface, system
Cucurbituril [7] Studies of Fluorescent Film Sensors is obtained, during preparation, gently to put the first step silicon when operation in step (3)
Then the quartz glass plate of alkanisation will be squeezed gently, prevent from destroying quartz glass plate while also having reached the uniform mesh of solution layer
's.Cucurbituril [7] supermolecular film fluorescent optical sensor is put into when in use in quartz surfaces ware, is diagonally placed, be added to
Jamaicin or palmatine, the coptis aqueous slkali of survey, are put into fluorescence spectrophotometer range meter, using 350 nm as excitation wavelength, 500 nm
Left and right is that launch wavelength measures, and discovery has biggish fluorescence sensitivity.Before measuring next sample every time, it is only necessary to 0.01
mol·L–1NaOH solution is rinsed, then is rinsed with secondary distilled water to unstressed configuration, and next sample can be measured.
When developing Cucurbituril [7] Studies of Fluorescent Film Sensors, while it also tested Cucurbituril [7], methyl methacrylate
Influence of the amount of ester and DMF solution (n,N-Dimethylformamide solution) to thin film sensor performance, methyl methacrylate
Dosage is excessive, thin film sensor not easy cleaning.
Compared with prior art the invention has the following advantages: the Cucurbituril of method provided by the present invention preparation
[7] Studies of Fluorescent Film Sensors finds that fluorescence is aobvious for the measurement of the morphinane alkaloids sample such as jamaicin, palmatine, coptisine
Enhancing is write, and is in good linear relationship；And it can be used for the measurement of these practical drugs and biological sample.With it is existing homogeneous glimmering
Optical sensor is compared, have many advantages, such as performance it is stable, it is reusable, do not pollute system to be measured, be simplicity, quick, and be expected to reality
Existing device production and automatic assay.
Detailed description of the invention
Fig. 1 is the fluorescence spectra of the palmatine of Cucurbituril [7] Studies of Fluorescent Film Sensors various concentration.
Fig. 2 is the shows fluorescent microscopy images of Cucurbituril [7] Studies of Fluorescent Film Sensors.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
A kind of preparation method of Cucurbituril [7] Studies of Fluorescent Film Sensors, includes the following steps:
(1) by quartz glass plate in dense H2SO4With 30% H2O2Mixture (volume ratio 7:3) Piranha etching liquid in impregnate 72
H removes the organic matter on surface；Place into 2 molL–1NaOH solution in impregnate 6 ~ 8 h, thoroughly neutralize the acid on surface, allow stone
The hydroxyl of English glass sheet surface is completely exposed；Quartz glass plate is then taken out, with a large amount of distilled water flushing surface, until clean
Only；Quartz glass plate is put into 1 molL again–1Methacrylic acid 3-(trimethoxy silane) propyl ester silane finish aqueous solution
In, impregnate 12 h；
(2) the allyloxy Cucurbituril [7] of 0.04 g(0.02 mmol) is added 3 mLN, in dinethylformamide solution,
Add 3 mL(28.3 mmol) in the DMF solution of methyl methacrylate monomer, the benzophenone light for adding 0.05g draws
Hair agent and 1g benzoin ethyl ether photosensitizer, 15 min of ultrasound are mixed them thoroughly；
(3) well-mixed solution drop is put into the quartz glass plate of first step silanization on polyfluortetraethylene plate, squeezed,
Keep the solution layer below sheet glass uniform, there cannot be bubble；Photoinitiated reactions, reaction 2 are carried out with the ultraviolet lighting of 254 nm
After h, quartz glass plate is sequentially placed into water, 15 min of ultrasound in ethyl alcohol, is rinsed with secondary distilled water, in quartz glass plate table
Face forms one layer of uniform film, obtains Cucurbituril [7] Studies of Fluorescent Film Sensors.
The present embodiment characterizes Cucurbituril [7] Studies of Fluorescent Film Sensors using fluorescence microscopy: because of Cucurbituril
[7] stable inclusion compound can be formed with spermine, spermine is reacted with fluorescein isothiocynate (aqueous solution of molar ratio 1:1), made
At spermine-fluorescein isothiocynate fluorescent marker.With blank assay counter point, by Cucurbituril [7] Studies of Fluorescent Film Sensors stone
Blank quartz slide (as other experiment conditions, allyloxy Cucurbituril [7] are only not added) made from English slide and same method into
Row comparison.Quartz slide immerses in spermine-fluorescein isothiocynate aqueous solution, impregnates several minutes, is rinsed with water after immersion.With glimmering
Light microscope observation, the results showed that the visible uniform yellow in Cucurbituril [7] Studies of Fluorescent Film Sensors quartz slide surface is glimmering
Luminous point, and blank control quartz glass plate is then without yellow fluorescence point.Fluorescent Characterization figure is shown in Fig. 1.
Cucurbituril made from the present embodiment [7] thin film sensor is put into quartz surfaces ware, is diagonally placed, be added to
Jamaicin or palmatine, the coptis aqueous slkali of survey, are put into fluorescence spectrophotometer range meter, using 350 nm as excitation wavelength, 500 nm
Left and right is that launch wavelength measures, and discovery has biggish fluorescence sensitivity.Before measuring next sample every time, it is only necessary to 0.01
mol·L–1NaOH solution is rinsed, then is rinsed with secondary distilled water to unstressed configuration, and next sample can be measured.
In practical measurement, the concentration of palmatine or jamaicin, coptisine stock solution is 1.0 × 10–4 mol·L–1.Make
It is diluted with preceding with secondary distilled water, adds 1 molL–1HCl adjust pH value be 1.Palmatine is passed in Cucurbituril [7] film fluorescence
Fluorescence spectra on sensor is shown in Fig. 2, and the concentration of palmatine is followed successively by (× 10–5 mol·L–1): (a) 0.4; (b) 0.5;
(c) 0.6; (d) 0.7; (e) 0.8; (f) 0.9; (g) 1.0; (h) 1.1; (i) 1.2; (j) 1.6; (k)
2.0.As can be seen from Figure 2 with the increase of palmatine concentration, fluorescence intensity is gradually increased.Palmatine or jamaicin, the coptis
Good linear relationship is presented in the concentration of alkali three and the relationship of fluorescence intensity respectively.Jamaicin, palmatine and coptisine are linear
Equation is respectively Y=8.07 × 106X+28.20(0.1 ~ 1.1 × 10–5 mol·L–1)；Y=8.36×106X+30.15(0.1 ~ 1.2
×10–5 mol·L–1)；Y=6.56×106X+22.34(0.2 ~ 1.3 × 10–5 mol·L–1).Y is fluorescence intensity, and X is solution
Concentration.
The scope of protection of present invention is not limited to the above specific embodiment, and for those skilled in the art and
Speech, the present invention can there are many deformation and change, it is all within design and principle of the invention it is made it is any modification, improve and
Equivalent replacement should be all included within protection scope of the present invention.
Claims (2)
1. a kind of preparation method of Cucurbituril [7] Studies of Fluorescent Film Sensors, characterized by the following steps:
(1) quartz glass plate is impregnated to 48 ~ 96 h in Piranha etching liquid, removes the organic matter on surface；Place into 1.5-2.5
mol·L–1NaOH solution in impregnate 6 ~ 8 h, thoroughly neutralize surface acid, allow the hydroxyl on quartz glass plate surface to be completely exposed；
Quartz glass plate is then taken out, with distilled water flushing surface, until clean；Quartz glass plate is put into 1 ~ 1.5 molL again–1
Methacrylic acid 3-(trimethoxy silane) in propyl ester silane finish aqueous solution, impregnate 11 ~ 14 h；
(2) a certain amount of allyloxy Cucurbituril [7] is added in n,N-Dimethylformamide solution, is then added a certain amount of
In the n,N-Dimethylformamide solution of methyl methacrylate monomer, a certain amount of diphenyl ketone photo initiator and peace are added
Fragrant ether photosensitizer is ceased, 15 min of ultrasound are mixed them thoroughly；
(3) well-mixed solution drop is put into the quartz glass plate of first step silanization on polyfluortetraethylene plate, squeezed,
Keep the solution layer below sheet glass uniform, there cannot be bubble；Photoinitiated reactions are carried out with the ultraviolet lighting of 254 nm, are reacted
After 1.5 ~ 2.5 h, quartz glass plate is sequentially placed into water, 15 ~ 20 min of ultrasound in ethyl alcohol, is rinsed with secondary distilled water,
Quartz glass plate surface forms one layer of uniform film, obtains Cucurbituril [7] Studies of Fluorescent Film Sensors.
2. a kind of preparation method of Cucurbituril [7] Studies of Fluorescent Film Sensors according to claim 1, it is characterised in that: step
Suddenly in (2), the allyloxy Cucurbituril [7] of 0.04 g is added in the n,N-Dimethylformamide solution of 3 mL, is then added 3
In the n,N-Dimethylformamide solution of the methyl methacrylate monomer of mL, add 0.05 g diphenyl ketone photo initiator and
1 g benzoin ethyl ether photosensitizer, 15 min of ultrasound are mixed them thoroughly.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070092867A1 (en) * | 2005-10-20 | 2007-04-26 | Postech Foundation | Application using non-covalent bond between a cucurbituril derivative and a ligand |
| US20070224403A1 (en) * | 2004-04-21 | 2007-09-27 | Postech Academy-Industry Foundation | Ultrathin Polymer Film Using Cucurbituril Derivative and Method of Forming the Same |
| CN101792115A (en) * | 2010-03-16 | 2010-08-04 | 清华大学 | Cucurbituril subject-object based chemical nano structure membrane and preparation method and application thereof |
-
2019
- 2019-05-26 CN CN201910443081.5A patent/CN110082333A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070224403A1 (en) * | 2004-04-21 | 2007-09-27 | Postech Academy-Industry Foundation | Ultrathin Polymer Film Using Cucurbituril Derivative and Method of Forming the Same |
| US20070092867A1 (en) * | 2005-10-20 | 2007-04-26 | Postech Foundation | Application using non-covalent bond between a cucurbituril derivative and a ligand |
| CN101792115A (en) * | 2010-03-16 | 2010-08-04 | 清华大学 | Cucurbituril subject-object based chemical nano structure membrane and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 段学超: "葫芦脲化学传感器的制备及其分子识别作用", 《中国优秀硕士学位论文全文数据库 信息科技辑》 * |
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