CN102507515A - Fluorescent ion imprint sensor for detection of cadmium ions and preparation method thereof - Google Patents
Fluorescent ion imprint sensor for detection of cadmium ions and preparation method thereof Download PDFInfo
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- CN102507515A CN102507515A CN2011102986685A CN201110298668A CN102507515A CN 102507515 A CN102507515 A CN 102507515A CN 2011102986685 A CN2011102986685 A CN 2011102986685A CN 201110298668 A CN201110298668 A CN 201110298668A CN 102507515 A CN102507515 A CN 102507515A
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Abstract
The invention provides a fluorescent ion imprint sensor for selective detection of cadmium ions and a preparation method of the fluorescent ion imprint sensor. The preparation method for the sensor comprises the steps of: preassembling the cadmium ions and functional monomers and fluorescent matters; then adding a cross-linking agent and an initiating agent, and taking a microporous filter membrane as a supporting medium; photo-thermally initiating and polymerizing to form a film; and eluting by acid and EDTA (Ethylene Diamine Tetraacetic Acid) to obtain the fluorescent cadmium ion imprint composite membrane sensor. The obtained imprint composite membrane has high selectivity and sensitivity for the cadmium ions and can be recycled for multiple times; and the fluorescent sensor provided by the invention is simple and quick to prepare and can be used for selective detection of the cadmium ions in an environment and other samples.
Description
(1) technical field
The present invention relates to a kind of fluorescence ion blotting sensor that is used for the cadmium ion detection and preparation method thereof.
(2) background technology
Cadmium ion is big to humans and animals toxicity, to system's toxigenicity effects such as kidney, lung, liver, bone and blood.Be used to detect the method such as the atomic absorption spectrography (AAS) of cadmium, electron probe, middle word activation and inductively coupled plasma mass spectrometry etc. all need large-scale instrument, detect loaded down with trivial detailsly, and cost is higher; In detection method commonly used, XRF becomes the focus of metal ion detection because of its advantage such as easy, quick.The classical organic fluorescence identification system that research at present is more, like the synthetic recognition system of genus experiences such as crown ether, calixarenes, synthesis step is loaded down with trivial details; Time-consuming, effort, synthetic acceptor are difficult to guarantee single-minded identity, and bio-identification systems such as DNA or albumen; Also exist cost an arm and a leg, life-span shortage point; Be not suitable for severe rugged environments such as high temperature, high pressure, and can not reuse, press for that development and preparation is simple, good stability, life-span are long, be prone to the selectivity cadmium ion fluorescent optical sensor preserved.
The ion blotting technology adopts the ion imprinted polymer of metallic ion as the template preparation; Have advantages such as single-minded recognition site, high anti-interference and anti-extraneous mal-condition; Can be applicable to the compartment analysis of metallic ion in SPE and the actual sample, but the report that is applied to the fluorescent optical sensor field seldom.The high selectivity and the highly sensitive of fluorescent technique of ion blotting technology are combined, and the cadmium ion trace fluorescent optical sensor of acquisition has characteristics such as selectivity is good, preparation is simple, the life-span is long, and can repeatedly recycle, and is easy to combine with optical device.
(3) summary of the invention
The object of the invention provide a kind ofly prepare that simple, good stability, life-span are long, the selectivity cadmium ion fluorescent optical sensor that is prone to preserve and preparation method thereof and analytical applications.
The technical scheme that the present invention adopts is:
A kind of fluorescence ion blotting sensor that is used for the cadmium ion detection is prepared by following method:
(1) cadmium ion and fluorescent chemicals are dissolved in solvent and assemble in advance, and then add function monomer, crosslinking chemical and initiating agent and mix;
Said fluorescent chemicals is thiooxine and 2-naphthyl acrylic ester;
Said function monomer is one of following: methacrylic acid, acrylic acid, 2-vinylpyridine, 4-vinylpridine, acrylic amide;
Said crosslinking chemical is one of following or its potpourri: ethylene glycol dimethacrylate, trimethoxy
Base propane trimethyl acrylic acid;
Said initiating agent is an azoisobutyronitrile;
(2) place step (1) reaction solution to keep 10～60min miillpore filter, take out miillpore filter then and be sandwiched in deaeration between glass plate or quartz plate, the degassing and sealing;
Said miillpore filter is vinylidene fluoride film or CAM;
(3) step (2) miillpore filter is carried out polyreaction 6～32 hours down or in 60～70 ℃ of water-baths in ultraviolet light, make blotting membrane;
(4) with the cadmium ion on the eluent wash-out blotting membrane, promptly get said fluorescence ion blotting sensor, said eluent is one of following: acetic acid, hydrochloric acid, sulfuric acid, nitric acid or EDTA.
Cadmium ion trace sensor of the present invention is the macromolecule type sensor that multiple function monomer and fluorescent chemicals polymerization form, and according to the characteristics that the ion blotting precordainment " is cut the garment according to the figure ", regulates part and arranges in order; To customize exclusive 3 D stereo opening structure, realize single-minded identification through " intelligent memory " substrate, can compare favourably with natural biological recognition system to the target heavy metal; Also have the following advantages simultaneously: preparation is simple relatively, good stability, be prone to preserve; Life-span is long, can repeatedly recycle, and does not pollute sample; And be easy to combine with optical device, have extensive practicality.
The invention still further relates to a kind of method for preparing said fluorescence ion blotting sensor, said method comprises:
(1) cadmium ion and fluorescent chemicals are dissolved in solvent and assemble in advance, and then add function monomer, crosslinking chemical and initiating agent and mix;
Said fluorescent chemicals is thiooxine and 2-naphthyl acrylic ester;
Said function monomer is one of following: methacrylic acid, acrylic acid, 2-vinylpyridine, 4-vinylpridine, acrylic amide;
Said crosslinking chemical is one of following or its potpourri: ethylene glycol dimethacrylate, trimethoxy propane trimethyl acrylic acid;
Said initiating agent is an azoisobutyronitrile;
(2) place step (1) reaction solution to keep 10～60min miillpore filter, take out miillpore filter then and be sandwiched in deaeration between glass plate or quartz plate, the degassing and sealing;
Said miillpore filter is vinylidene fluoride film or CAM;
(3) step (2) miillpore filter is carried out polyreaction 6～32 hours down or in 60～70 ℃ of water-baths in ultraviolet light, make blotting membrane;
(4) with the cadmium ion on the eluent wash-out blotting membrane, promptly get said fluorescence ion blotting sensor, said eluent is one of following: acetic acid, hydrochloric acid, sulfuric acid, nitric acid or EDTA.(5) cadmium ion, fluorescent chemicals and function monomer consumption mol ratio are in the said step (1): 1: 1～3: 4～320, and function monomer and dosage of crosslinking agent mol ratio are: 1: 2～8.
(6) initiator solution concentration is preferably 0.005～0.02g/ml in the said step (2).
The invention still further relates to the application of described high molecular fluorescent ion blotting sensor in cadmium ion detects.Concrete application process is following:
At first fluorescence trace wet film (dry film is abundant swelling in ionized water) is positioned in the fluorescence orifice plate.With sample solution warp 0.45 μ m filtering with microporous membrane; Add HCl-Tris buffer solution regulator solution pH=7 then; Get the above-mentioned solution of 300 μ l and add mensuration fluorescence intensity variation in the fluorescence microwell plate that contains the fluorescence blotting membrane, establishing criteria sample calibration curve carries out measurement of concetration.
Beneficial effect of the present invention is mainly reflected in: the invention provides a kind of fluorescence ion blotting sensor that cadmium ion detects that is used for; Its form is a macromolecule membrane; The preparation process is simple relatively, good stability, life-span are long, be prone to preserve; And can recycle repeatedly performance and do not change, have extensive practicality, be the simple and direct method fast that solves heavy metal ion high selectivity, high-sensitivity detection.
(4) description of drawings
Fig. 1 is embodiment 8 canonical plottings.
(5) embodiment
Below in conjunction with specific embodiment the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1:
With 0.01mmol 2-naphthyl acrylic ester and 0.005mmol template ion (Cd
2+) in 1.5mlDMSO, mix and stir 30min, add 2-vinylpyridine 1.6mmol again, 8mmol ethylene glycol dimethacrylate crosslinking chemical and 0.03g azoisobutyronitrile, ultrasonic mixing 30min; 0.45 μ m vinylidene fluoride film takes out after placing above-mentioned mixed solution to leave standstill 20min, clamps with sealing film sealing back 65 ℃ of following water-bath heating 7 hours with quartz plate, makes cadmium fluorescence blotting membrane (being cadmium ion fluorescence trace sensor).0.1M HNO
3Template ion on the eluant solution blotting membrane is stable until fluorescence intensity, and with the residual HNO of ultrapure water eccysis
3After, with the blotting membrane drying for standby.Gained fluorescence trace biosensor analysis detects the best pH=7 of cadmium ion, and it is constant to recycle life-span 20 performances.
Embodiment 2:
With 0.005mmol template ion (Cd
2+) and 0.01mmol 2-naphthyl acrylic ester be dissolved among the 2ml DMSO mixing and stir 30min, add 4-vinylpridine 1.0mmol again, 4mmol trimethoxy propane trimethyl acrylic acid and 0.01g azoisobutyronitrile, ultrasonic mixing 20min; Take out after placing above-mentioned mixed solution to leave standstill 20min the 0.45 μ m vinylidene fluoride film, clamp with sealing film sealing back, make cadmium ion fluorescence trace sensor 65 ℃ of following water-baths heating 10 hours with quartz plate.Use 0.1M HNO
3Template ion on the eluant solution blotting membrane is stable until fluorescence intensity, and with the residual HNO of ultrapure water eccysis
3After, with the blotting membrane drying for standby.Gained fluorescence trace biosensor analysis detects the best pH=7 of cadmium ion, and it is constant to recycle life-span 20 performances.
Embodiment 3:
With 0.01mmol thiooxine and 0.005mmol template ion (Cd
2+) be dissolved in to mix among the 1.5mlDMSO and stir 20min; In said mixture, add the 0.1mmol methacrylic acid, 0.8mmol ethylene glycol dimethacrylate and 0.01g azoisobutyronitrile fully mix, ultrasonic mixing 30min; Take out after placing above-mentioned solution to leave standstill 30min the 0.45 μ m CAM, clamp, drive out of behind the bubble with sealing film sealing back 65 ℃ of following water-baths heating 15 hours with quartz plate.After reacting completely, with the metallic ion blotting membrane of preparation earlier with behind the EDTA with 0.1M HCl eluant solution template ion, until the fluorescence intensity vary stable, with the residual HCl of ultrapure water eccysis, then with the blotting membrane drying for standby.Gained fluorescence trace biosensor analysis detects the best pH=7 of cadmium ion, and it is constant to recycle life-span 20 performances.
Embodiment 4:
With 0.015mmol thiooxine and 0.005mmol template ion (Cd
2+) be dissolved in to mix among the 1.5ml DMSO and stir 20min; In said mixture, add the 1mmol acrylic amide, 5mmol ethylene glycol dimethacrylate and 0.015g azoisobutyronitrile fully mix, ultrasonic mixing 30min; Take out after placing above-mentioned solution to leave standstill 20min the 0.45 μ m vinylidene fluoride film, clamp, drive bubble sealing back out of and under ultra violet lamp, reacted 24 hours with quartz plate.After reacting completely, that the metallic ion blotting membrane of preparation is first with 0.1M sulfuric acid solution wash-out template ion, until the fluorescence intensity vary stable, with the residual acid of ultrapure water eccysis, then with the blotting membrane drying for standby.Gained fluorescence trace biosensor analysis detects the best pH=7 of cadmium ion, and it is constant to recycle life-span 20 performances.
Embodiment 5:
With 0.005mmol template ion (Cd
2+) and 0.02mmol 2-naphthyl acrylic ester be dissolved in 2ml DMSO and 1mlH
2Stir 15min in the O mixed solution, add 2-vinylpyridine 1.2mmol again, 4mmol trimethoxy propane trimethyl acrylic acid and 0.01g azoisobutyronitrile, ultrasonic mixing 20min; Take out after placing above-mentioned mixed solution to leave standstill 15min the 0.45 μ m vinylidene fluoride film, clamp degassing sealing back with quartz plate and under ultra violet lamp, reacted 32 hours, make cadmium ion fluorescence trace sensor.Use 0.1M HNO
3Template ion on the eluant solution blotting membrane is stable until fluorescence intensity, and with the residual HNO of ultrapure water eccysis
3After, with the blotting membrane drying for standby.Gained fluorescence trace biosensor analysis detects the best pH=7 of cadmium ion, and it is constant to recycle life-span 20 performances.
Embodiment 6:
With 0.02mmol thiooxine and 0.02mmol template ion (Cd
2+) be dissolved in to mix among the 2mlDMSO and stir 10min; In said mixture, add the 0.8mmol methacrylic acid, 1.6mmol trimethoxy propane trimethyl acrylic acid and 0.01g azoisobutyronitrile fully mix, ultrasonic mixing 35min; Take out after placing above-mentioned solution to leave standstill 20min the 0.45 μ m vinylidene fluoride film, clamp, drive out of behind the bubble with sealing film sealing back 65 ℃ of following water-baths heating 20 hours with quartz plate.After reacting completely, the metallic ion blotting membrane of preparation is first with EDTA eluant solution template ion, until the fluorescence intensity vary stable, and with behind the residual EDTA of ultrapure water eccysis, with the blotting membrane drying for standby.Gained fluorescence trace biosensor analysis detects the best pH=7 of cadmium ion, and it is constant to recycle life-span 20 performances.
Embodiment 7:
With 0.01mmol 2-naphthyl acrylic ester and 0.005mmol template ion (Cd
2+) in 1.5mlDMSO, mix and stir 30min, add 2-vinylpyridine 1.6mmol again, 8mmol ethylene glycol dimethacrylate crosslinking chemical and 0.03g azoisobutyronitrile, ultrasonic mixing 30min; 0.45 μ m vinylidene fluoride film takes out after placing above-mentioned mixed solution to leave standstill 20min, clamps with sealing film sealing back 65 ℃ of following water-bath heating 7 hours with quartz plate, makes cadmium fluorescence blotting membrane (being cadmium ion fluorescence trace sensor).0.1M HNO
3Template ion on the eluant solution blotting membrane is stable until fluorescence intensity, and with the residual HNO of ultrapure water eccysis
3After, with the blotting membrane drying for standby.Gained fluorescence trace biosensor analysis detects the best pH=7 of cadmium ion, and it is constant to recycle life-span 20 performances.
Embodiment 8: the application implementation example
Typical curve is drawn: get ultrapure water and add the gradient concentration cadmium ion; Be adjusted to the standard solution of pH=7 then with HCl-Tris buffer solution; The fluorescence trace wet film that embodiment 1 is made is positioned in the fluorescence orifice plate; Adding 300 μ l standard solutions and measure the fluorescence intensity (the fluorescence trace wet film fluorescence intensity that adds standard solution is designated as I) that adds cadmium ion front and back fluorescence trace wet film, is that contrast (is designated as I with the fluorescence trace wet film that does not add cadmium ion
0), with the standard solution concentration of cadmium ions be horizontal ordinate, with (I/I
0-1) % is an ordinate, drawing standard curve (referring to Fig. 1).
The actual water sample cadmium ion detects: get the river water sample through 0.45 μ m filtering with microporous membrane, add HCl-Tris buffer solution regulator solution pH=7 then.The fluorescence trace dry film that embodiment 1 is made fully is positioned in the fluorescence orifice plate after the swelling in deionized water; Getting the above-mentioned solution of 300 μ l adds in the fluorescence microwell plate that contains the fluorescence blotting membrane and measures fluorescence intensity; The reference standard curve; Record water sample and contain cadmium ion 0.14mg/l (with adopting inductively coupled plasma mass spectrometry mensuration basically identical as a result), the recovery of actual water sample is between 98%～103%.
Claims (5)
1. one kind is used for the fluorescence ion blotting sensor that cadmium ion detects, and is prepared by following method:
(1) cadmium ion and fluorescent chemicals are dissolved in solvent and assemble in advance, and then add function monomer, crosslinking chemical and initiating agent and mix;
Said fluorescent chemicals is thiooxine and 2-naphthyl acrylic ester;
Said function monomer is one of following: methacrylic acid, acrylic acid, 2-vinylpyridine, 4-vinylpridine, acrylic amide;
Said crosslinking chemical is one of following or its potpourri: ethylene glycol dimethacrylate, trimethoxy propane trimethyl acrylic acid;
Said initiating agent is an azoisobutyronitrile;
(2) place step (1) reaction solution to keep 10～60min miillpore filter, take out miillpore filter then and be sandwiched in deaeration between glass plate or quartz plate, the degassing and sealing;
Said miillpore filter is vinylidene fluoride film or CAM;
(3) step (2) miillpore filter is carried out polyreaction 6～32 hours down or in 60～70 ℃ of water-baths in ultraviolet light, make blotting membrane;
(4), promptly get said fluorescence ion blotting sensor with the cadmium ion on the eluent wash-out blotting membrane.
2. method for preparing the said fluorescence ion blotting of claim 1 sensor, said method comprises:
(1) cadmium ion and fluorescent chemicals are dissolved in solvent and assemble in advance, and then add function monomer, crosslinking chemical and initiating agent and mix;
Said fluorescent chemicals is thiooxine and 2-naphthyl acrylic ester;
Said function monomer is one of following: methacrylic acid, acrylic acid, 2-vinylpyridine, 4-vinylpridine, acrylic amide;
Said crosslinking chemical is one of following or its potpourri: ethylene glycol dimethacrylate, trimethoxy propane trimethyl acrylic acid;
Said initiating agent is an azoisobutyronitrile;
(2) place step (1) reaction solution to keep 10～60min miillpore filter, take out miillpore filter then and be sandwiched in deaeration between glass plate or quartz plate, the degassing and sealing;
Said miillpore filter is vinylidene fluoride film or CAM;
(3) step (2) miillpore filter is carried out polyreaction 6～32 hours down or in 60～70 ℃ of water-baths in ultraviolet light, make blotting membrane;
(4) with the cadmium ion on the eluent wash-out blotting membrane, promptly get said fluorescence ion blotting sensor, said eluent is one of following: acetic acid, hydrochloric acid, sulfuric acid, nitric acid or EDTA.
3. method as claimed in claim 2 is characterized in that cadmium ion, fluorescent chemicals and function monomer consumption mol ratio are in the said step (1): 1: 1～3: 4～320, and function monomer and dosage of crosslinking agent mol ratio are: 1: 2～8.
4. method as claimed in claim 2 is characterized in that initiator solution concentration is 0.005～0.02g/ml in the said step (2).
5. the application of the described fluorescence ion blotting of claim 1 sensor in cadmium ion detects.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103254354A (en) * | 2013-05-24 | 2013-08-21 | 福州大学 | Cadmium ion imprinted adsorbent, and preparation method and application thereof |
| CN106256839A (en) * | 2015-06-18 | 2016-12-28 | 中国石油化工股份有限公司 | A kind of method that ion blotting composite membrane is prepared in surface heat polymerization |
| CN106256414A (en) * | 2015-06-18 | 2016-12-28 | 中国石油化工股份有限公司 | A kind of preparation method of the hollow fiber film assembly of Selective Separation metal ion |
| CN108445053A (en) * | 2018-02-26 | 2018-08-24 | 江苏大学 | A kind of ion blotting sensor and preparation method and application |
| CN109351347A (en) * | 2018-09-28 | 2019-02-19 | 昆明理工大学 | It is a kind of using acrylamide as the preparation method and application of the hexavalent chromium trace composite membrane of function monomer |
| CN109589943A (en) * | 2018-12-03 | 2019-04-09 | 昆明理工大学 | A method of preparing cadmium (II) ion blotting composite membrane |
| CN109589799A (en) * | 2018-12-03 | 2019-04-09 | 昆明理工大学 | A kind of preparation method of cadmium (II) ion blotting composite membrane |
| CN112611785A (en) * | 2020-11-26 | 2021-04-06 | 北京信息科技大学 | Field-effect tube micro sensor and preparation method and application thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103254354A (en) * | 2013-05-24 | 2013-08-21 | 福州大学 | Cadmium ion imprinted adsorbent, and preparation method and application thereof |
| CN103254354B (en) * | 2013-05-24 | 2016-03-09 | 福州大学 | A kind of cadmium ion trace sorbent material and its preparation method and application |
| CN106256414B (en) * | 2015-06-18 | 2019-05-31 | 中国石油化工股份有限公司 | A kind of preparation method of the hollow fiber film assembly of Selective Separation metal ion |
| CN106256414A (en) * | 2015-06-18 | 2016-12-28 | 中国石油化工股份有限公司 | A kind of preparation method of the hollow fiber film assembly of Selective Separation metal ion |
| CN106256839B (en) * | 2015-06-18 | 2019-02-19 | 中国石油化工股份有限公司 | A kind of method that surface thermal polymerization prepares ion blotting composite membrane |
| CN106256839A (en) * | 2015-06-18 | 2016-12-28 | 中国石油化工股份有限公司 | A kind of method that ion blotting composite membrane is prepared in surface heat polymerization |
| CN108445053A (en) * | 2018-02-26 | 2018-08-24 | 江苏大学 | A kind of ion blotting sensor and preparation method and application |
| CN109351347A (en) * | 2018-09-28 | 2019-02-19 | 昆明理工大学 | It is a kind of using acrylamide as the preparation method and application of the hexavalent chromium trace composite membrane of function monomer |
| CN109589943A (en) * | 2018-12-03 | 2019-04-09 | 昆明理工大学 | A method of preparing cadmium (II) ion blotting composite membrane |
| CN109589799A (en) * | 2018-12-03 | 2019-04-09 | 昆明理工大学 | A kind of preparation method of cadmium (II) ion blotting composite membrane |
| CN109589799B (en) * | 2018-12-03 | 2021-10-22 | 昆明理工大学 | Preparation method of cadmium (II) ion imprinting composite membrane |
| CN109589943B (en) * | 2018-12-03 | 2021-11-12 | 昆明理工大学 | Method for preparing cadmium (II) ion imprinting composite membrane |
| CN112611785A (en) * | 2020-11-26 | 2021-04-06 | 北京信息科技大学 | Field-effect tube micro sensor and preparation method and application thereof |
| CN112611785B (en) * | 2020-11-26 | 2022-11-08 | 北京信息科技大学 | Field-effect tube micro sensor and preparation method and application thereof |
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Application publication date: 20120620 |