CN106010512A - SiO2/Au nano composite material used for Hg2<+> detection and preparation method thereof - Google Patents
SiO2/Au nano composite material used for Hg2<+> detection and preparation method thereof Download PDFInfo
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- CN106010512A CN106010512A CN201610308709.7A CN201610308709A CN106010512A CN 106010512 A CN106010512 A CN 106010512A CN 201610308709 A CN201610308709 A CN 201610308709A CN 106010512 A CN106010512 A CN 106010512A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 140
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 73
- 239000000463 material Substances 0.000 title claims abstract description 64
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 63
- 238000001514 detection method Methods 0.000 title claims abstract description 43
- 229910052681 coesite Inorganic materials 0.000 title claims abstract description 41
- 229910052906 cristobalite Inorganic materials 0.000 title claims abstract description 41
- 229910052682 stishovite Inorganic materials 0.000 title claims abstract description 41
- 229910052905 tridymite Inorganic materials 0.000 title claims abstract description 41
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000010931 gold Substances 0.000 claims abstract description 122
- 229910052737 gold Inorganic materials 0.000 claims abstract description 43
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 238000001338 self-assembly Methods 0.000 claims abstract description 15
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- 229910000077 silane Inorganic materials 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims abstract description 3
- BQPIGGFYSBELGY-UHFFFAOYSA-N mercury(2+) Chemical compound [Hg+2] BQPIGGFYSBELGY-UHFFFAOYSA-N 0.000 claims description 59
- 108090000765 processed proteins & peptides Proteins 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 18
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims description 17
- MCEBKLYUUDGVMD-UHFFFAOYSA-N [SiH3]S(=O)=O Chemical compound [SiH3]S(=O)=O MCEBKLYUUDGVMD-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 229960003180 glutathione Drugs 0.000 claims description 12
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 8
- 230000004044 response Effects 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 108010024636 Glutathione Proteins 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Natural products NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 4
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims description 4
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 claims description 3
- 239000004475 Arginine Substances 0.000 claims description 3
- 239000004471 Glycine Substances 0.000 claims description 3
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical group C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 3
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 claims description 3
- HNDVDQJCIGZPNO-YFKPBYRVSA-N L-histidine Chemical compound OC(=O)[C@@H](N)CC1=CN=CN1 HNDVDQJCIGZPNO-YFKPBYRVSA-N 0.000 claims description 3
- ROHFNLRQFUQHCH-YFKPBYRVSA-N L-leucine Chemical group CC(C)C[C@H](N)C(O)=O ROHFNLRQFUQHCH-YFKPBYRVSA-N 0.000 claims description 3
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 claims description 3
- ROHFNLRQFUQHCH-UHFFFAOYSA-N Leucine Chemical group CC(C)CC(N)C(O)=O ROHFNLRQFUQHCH-UHFFFAOYSA-N 0.000 claims description 3
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004472 Lysine Substances 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- 235000004279 alanine Nutrition 0.000 claims description 3
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims description 3
- HNDVDQJCIGZPNO-UHFFFAOYSA-N histidine Natural products OC(=O)C(N)CC1=CN=CN1 HNDVDQJCIGZPNO-UHFFFAOYSA-N 0.000 claims description 3
- 238000007689 inspection Methods 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 125000003630 glycyl group Chemical group [H]N([H])C([H])([H])C(*)=O 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 54
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 239000011259 mixed solution Substances 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 24
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- 238000002189 fluorescence spectrum Methods 0.000 description 5
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000004611 spectroscopical analysis Methods 0.000 description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 3
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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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
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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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"
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Abstract
The invention discloses a SiO2/Au nano composite material used for Hg2<+> detection and a preparation method thereof and belongs to the technical field of heavy metal ion detection. The prepared SiO2/Au nano composite material has high Hg2<+> detection sensitivity and can be repeatedly used. The preparation method includes the steps that 3-mercaptopropyltrimethoxysilane and a silicon dioxide precursor are added into an organic solvent and evenly stirred to obtain a silane mixed solution; the silane mixed solution is added into a one-dimensional short-peptide self-assembly solution and evenly mixed, the pH value of the solution is adjusted to a specific value, and centrifugation and washing are conducted after reaction is conducted for a certain period of time to obtain white precipitate; the white precipitate is dispersed in water and mixed with a nano gold solution, stirring reaction is conducted for a certain period of time at certain temperature, and the one-dimensional SiO2/Au nano composite material is obtained after centrifugation, washing and drying. The method can be used for preparing the SiO2/Au nano composite material used for Hg2<+> detection.
Description
Technical field
The present invention relates to a kind of detection of heavy metal ion technical field, Hg2+The SiO of response2/ Au composite,
Particularly to Hg in a kind of fluorescent spectrometry detection environment2+The SiO of concentration2The preparation of/Au nano composite material
Method.
Background technology
Mercury ion (Hg2+) it is one of poisonous heavy metal ion, the mercury ion in environment can pass through food chain
Enrichment, finally at people's cylinder accumulation, causes brain and the damage of nervus centralis, kidney failure, DNA destruction
Deng, the health and lives of the mankind is caused serious threat (see Clarkson T.W. etc., " toxicology comment ",
2006,36:609).Therefore by simple and the method for economy accurately detects the mercury content in environment, for
Environmental warning and protection human health have great importance.
It is currently used for Hg2+The method of detection has atomic fluorescence method, cold-vapour atomic absorption method, inductively coupled plasma
Body constitution spectral analysis technology, colorimetry, fluorescent spectrometry etc..Compared to other several detection methods, fluorescence light
Spectrometry has highly sensitive, and selectivity is good, few by sample amount, method is easy, working curve range of linearity width etc.
Advantage, have broad application prospects in mercury ion detecting field (see Xu Yue etc., " analytical chemistry ",
2014,42:1252).
Nanometer gold is widely used at analysis detection field due to the Wuli-Shili-Renli system approach of its uniqueness.
Especially particle diameter is less than the gold grain of 5 nanometers, and quantum effect causes it to produce fluorescence when light excites, and
The wavelength launching fluorescence can regulate.This fluorescent characteristic of little granule nanometer gold can be used to detect in environment
The existence of mercury ion (see Fang C. etc., " research in nanotechnology bulletin ", 2010,5:1856).Common ion
In the binding ability of only hydrargyrum and sulfydryl exceeded the binding ability of gold and sulfydryl, the most this method notable
Advantage is strong interference immunity (sees Dingbin L. etc., " analytical chemistry ", 2010,82:9606).But this
The method of kind is typically disposable, is i.e. only used for one-time detection, causes the waste of resource.Exploitation can weigh
Utilize again, more highly sensitive detection method has important using value.
Summary of the invention
Based on this, it is an object of the invention to provide a kind of one-dimensional SiO2/ Au nano composite material and preparation side thereof
Method, repeatable is applied to heavy metal Hg2+Detection.
The invention provides a kind of for Hg2+The one-dimensional SiO of detection2The preparation method of/Au nano composite material,
Comprise the following steps:
1) in organic solvent, add hydrosulphonyl silane and silica precursor, stir, obtain silane and mix
Close solution；
2) silane mixture solution is joined in one-dimensional small peptide self assembly solution, mix homogeneously, regulate pH value of solution
To designated value, after reaction certain time, centrifugal, carrying out washing treatment, obtains white precipitate；
3) described white precipitate is dispersed in water, mixes with described nano-Au solution, stir under uniform temperature
Mix reaction certain time, by centrifugation, washing, dried, obtain one-dimensional SiO2/ Au nano composite material.
Optionally, during described hydrosulphonyl silane is mercaptopropyltriethoxysilane, mercaptopropyl trimethoxysilane
At least one, silica precursor is at least one in tetraethyl orthosilicate, methyl silicate, positive silicic acid,
Solvent is at least one in isopropanol, ethanol, methanol, acetone.
Preferably, described hydrosulphonyl silane is 1:2-1:20 with the ratio of silica precursor.
Optionally, described one-dimensional small peptide self assembly solution is prepared by the following method:
By the small peptide (X of certain massmYnType small peptide, X is glycine, alanine, leucine, different bright ammonia
At least one in acid, Y is at least one in lysine, arginine, histidine, and m is not more than 6, n
It is not more than 2) it is dissolved in the water, ultrasonic disperse, regulate to optimum pH, room temperature stands, obtains one-dimensional short
Peptide assembles solution.
Optionally, described nano-Au solution is prepared via a method which:
Take a certain amount of glutathione solution, chlorauric acid solution, ultra-pure water mixing, glutathion and gold chloride
Mol ratio be 1:5-1:30, at 30-90 DEG C react 1-12 hour, obtain glutathion protection nanometer gold
Solution.
Preferably, described white precipitate is 3-8 hour with the response time of nanometer gold, reaction temperature 10-40 DEG C.
A kind of for Hg2+The one-dimensional SiO of detection2/ Au nano composite material, including one-dimensional the two of sulfydryl modification
Silicon oxide and the nanometer gold that can launch fluorescence, when tested substance adds described SiO2In/Au solution, if
Tested substance contains Hg2+, the most described SiO2/ Au solution fluorescence emissive porwer reduces.
A kind of for Hg2+The one-dimensional SiO of detection2/ Au nano composite material, described nanometer gold and one-dimensional dioxy
Connected by sulfydryl between SiClx.
A kind of for Hg2+The one-dimensional SiO of detection2/ Au nano composite material, works as Hg2+Concentration is between 5-200
nmol L-1Time, described SiO2/ Au solution fluorescence emissive porwer and Hg2+Concentration has good linear relationship,
Therefore can be used for Hg2+Detection by quantitative.
A kind of for Hg2+The one-dimensional SiO of detection2/ Au nano composite material, can be repeated for Hg2+Detection.
The invention provides a kind of for Hg2+The one-dimensional SiO of detection2/ Au nano composite material and preparation side thereof
Method, compared with prior art, the present invention is by launching the nanometer gold of fluorescence and one-dimensional silicon dioxide
Combined by sulfydryl, keeping nanometer gold Fluorometric assay Hg2+While strong interference immunity, at tiny area
Improve the relative concentration of nanometer gold, the fluorescence intensity that being exaggerated reunites causes reduces phenomenon so that test knot
Fruit is more sensitive to the agglomeration of Au.Meanwhile, one-dimensional SiO2/ Au nano composite material is to Hg solution2+
There is enrichment effect, further increase Hg2+The sensitivity of detection.It addition, prepared one-dimensional SiO2/Au
Nano composite material radial dimension is nanoscale, and axial dimension has reached micron order, has bigger the most simultaneously
Contact response area and the feature of recyclable recycling, therefore have higher economic worth.
Accompanying drawing explanation
The one-dimensional SiO that Fig. 1 provides for the embodiment of the present invention2The transmission electron microscope of/Au nano composite material shines
Sheet；
The one-dimensional SiO that Fig. 2 provides for the embodiment of the present invention2The fluorescent emission spectrogram of/Au nano composite material (swashs
Sending out wavelength is 400nm)；
In the presence of Fig. 3 is different metal ion, the one-dimensional SiO that the embodiment of the present invention provides2The nano combined material of/Au
Fluorescence intensity level (B) at the fluorescent emission spectrogram (A) of material solution and 600nm；
The one-dimensional SiO that Fig. 4 provides for the embodiment of the present invention2/ Au Nanocomposite solution adds different hydrargyrum from
Fluorescent emission spectrogram during sub-concentration；
Fig. 5 is the relation curve (A) between the fluorescence intensity (600nm) and ion concentration of mercury obtained according to Fig. 4
With linear relationship scope (B)；
The one-dimensional SiO that Fig. 6 provides for the embodiment of the present invention2The fluorescence intensity of/Au Nanocomposite solution keeps
Coefficient and the relation curve recycling number of times.
Detailed description of the invention
Technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that
Described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are not making creative work premise
Lower obtained every other embodiment, broadly falls into the scope of protection of the invention.
Embodiments provide a kind of for Hg2+The one-dimensional SiO of detection2The system of/Au nano composite material
Preparation Method, comprises the following steps:
S1: add hydrosulphonyl silane and silica precursor in organic solvent, stir, obtain silane
Mixed solution.
In this step, the silica nanometer material being introduced for acquisition surface sulfydryl modification of hydrosulphonyl silane
Material, thus provide reliable anchored site to nanometer gold, and obtain SiO further2/ Au nano composite material.
In this step, first preparation is containing the precursor solution of the two.Concrete, by molten for the presoma of said two devices
In organic solvent, concrete, organic solvent is selected from methanol, ethanol, the tert-butyl alcohol and acetone at least
One, those skilled in the art can select voluntarily according to service condition.
S2: silane mixture solution is joined in one-dimensional small peptide self assembly solution, mix homogeneously, regulate solution
PH is to designated value, and after reaction certain time, centrifugal, carrying out washing treatment, obtains white precipitate；
In this step, one-dimensional small peptide self assembly solution can be catalyzed silane or silicon dioxide presoma hydrolysis and
Polycondensation reaction, and induce silicon dioxide or mercapto-functionalized silicon dioxide to deposit on small peptide self-assembly surface,
Obtain depending on the mercapto-functionalized silica nano material of assembly pattern.The pH of mineralising reaction is to product
The generating rate of thing, product morphology and structure have material impact, in the present embodiment, pH value 5-9 it
Between preferably, such as pH 5, pH 6, pH 7, pH 8, pH 9 all can prepare satisfactory one-dimensional dioxy
SiClx nano material.Concrete, silane mixture solution is added drop-wise in one-dimensional small peptide self assembly solution, mixing
Rear regulation, to suitable pH, obtains white precipitate by centrifugal, washing after having reacted.
S3: be dispersed in water by described white precipitate, mixes with described nano-Au solution, under uniform temperature
Stirring reaction certain time, by centrifugation, washing, dried, obtain one-dimensional SiO2/ Au nano composite material.
In this step, scattered nanometer gold by sulfydryl be anchored on one-dimensional silica nano fibrous on, many
Remaining nanometer gold, stabilizer etc. remove by the way of centrifugal and washing, and purification effect utilizes fluorescence emission
Spectrum is tested, until the fluorescence intensity of centrifuged supernatant is close to zero, obtains pure one after drying
Dimension SiO2/ Au nano composite material.
The invention provides a kind of for Hg2+The one-dimensional SiO of detection2/ Au nano composite material and preparation side thereof
Method, compared with prior art, the present invention is by launching the nanometer gold of fluorescence and one-dimensional silicon dioxide
Combined by sulfydryl, keeping nanometer gold Fluorometric assay Hg2+While strong interference immunity, at tiny area
Improve the relative concentration of nanometer gold, the fluorescence intensity that being exaggerated reunites causes reduces phenomenon so that test knot
Fruit is more sensitive to the agglomeration of Au.Meanwhile, one-dimensional SiO2/ Au nano composite material is to Hg solution2+
There is enrichment effect, further increase Hg2+The sensitivity of detection.It addition, prepared one-dimensional SiO2/Au
Nano composite material radial dimension is nanoscale, and axial dimension has reached micron order, has bigger the most simultaneously
Contact response area and the feature of recyclable recycling, therefore have higher economic worth.
In one embodiment of this invention, hydrosulphonyl silane is mercaptopropyltriethoxysilane, mercapto propyl group trimethoxy
At least one in base silane, silica precursor is in tetraethyl orthosilicate, methyl silicate, positive silicic acid
At least one, solvent is at least one in isopropanol, ethanol, methanol, acetone.The introducing of hydrosulphonyl silane
It is the 1-dimention nano silicon dioxide fibre in order to obtain surface sulfydryl modification, if but using simple sulfydryl silicon
Alkane, is difficult to obtain stable one-dimensional silica nano fibrous because its reactivity is low, therefore make its with
The one-dimensional silica nanometer that surface sulfydryl modification is prepared in the silica precursor copolycondensation of high reaction activity is fine
Dimension.It is to improve its dispersibility in water that hydrosulphonyl silane and silica precursor are firstly added solvent,
So that reaction can be carried out smoothly.Concrete, organic solvent can be chosen any one kind of them, and those skilled in the art can
Select the most voluntarily.
In one embodiment of this invention, hydrosulphonyl silane is 1:2-1:20 with the ratio of silica precursor.Two
The ratio of person is different, and speed, the structure of generated silicon dioxide and the surface sulfhydryl content of mineralising reaction have
Difference, it will be appreciated by persons skilled in the art that the silane mixture solution prepared within the above range
To meet the follow-up one-dimensional silica nano fibrous requirement preparing sulfydryl modification, can exist according to actual needs
Be adjusted in above-mentioned scope, such as 1:2,1:3,1:4,1:5,1:6,1:7,1:8,1:9,1:10,1:
11,1:12,1:13,1:14,1:15,1:16,1:17,1:18,1:19,1:20 etc..
In one embodiment of this invention, one-dimensional small peptide self assembly solution is prepared as follows: will be certain
Small peptide (the X of qualitymYnType small peptide, X be in glycine, alanine, leucine, isoleucine at least
One, Y is at least one in lysine, arginine, histidine, and m is not more than 6, and n is not more than 2)
It is dissolved in the water, ultrasonic disperse, regulate to optimum pH, room temperature stands, and obtains one-dimensional small peptide and assembles solution.
Amphipathic small peptide can pass through the drivings such as hydrophobic interaction, hydrogen bond, electrostatic interaction, molecular chiral and be assembled into a wiener
Rice structure, hydrophilic functional groups is distributed in the surface of assembly with stable assembly structure, meanwhile, this
A little functional groups have facilitation for the formation of silica silicon key, by such a molecule, are had
Having the one-dimensional small peptide self-assembly of catalysis mineralization ability, the deposition for follow-up silicon dioxide provides template and catalysis
Center.By hydrophilic amino acid and the change of hydrophobic amino acid, may be used to regulate self-assembly structure,
Size and surface nature etc..
In one embodiment of this invention, nano-Au solution is prepared in the following manner: take a certain amount of paddy Guang
Sweet peptide solution, chlorauric acid solution, ultra-pure water mix, and glutathion is 1:5-1:30 with the mol ratio of gold chloride,
React 1-12 hour at 30-90 DEG C, obtain the nano-Au solution of glutathion protection.In order to obtain can
Launch the nanometer gold of fluorescence, by glutathione reduction gold ion the nanometer gold that stably generates, prevent nanometer
Gold is reunited and is lost fluorescent emission ability.Concrete, first prepare certain density glutathione solution and chlorine
They are mixed with ultra-pure water by auric acid solution with the mol ratio of 1:5-1:30, react one the most at a certain temperature
Fix time.It will be appreciated by persons skilled in the art that the precursor solution of above-mentioned latitude of formulation all can be made
Standby nanometer gold, such as 1:5,1:10,1:15,1:20,1:25,1:30 etc., in addition, as long as paddy Guang
The mol ratio of sweet peptide and gold chloride is in the arbitrary value of above-mentioned scope.For the temperature and time of reaction,
In the application and be not specifically limited, it is common that the response time that temperature height needs is short, as long as can be had
There is the nanometer gold of fluorescent emission ability, whether synthetic effect fluorescence emission spectrum has obvious fluorescence
Emission peak is verified.
In one embodiment of this invention, white precipitate is 3-8 hour with the response time of nanometer gold, reaction temperature
Spend 10-40 DEG C.In the present embodiment, it is therefore an objective to free nanometer gold is connected to one-dimensional titanium dioxide by sulfydryl
On silicon nanofiber, the application is not specifically limited for concrete reaction temperature and time, and reaction effect is adopted
Verify with fluorescence emission spectrum.
A kind of for Hg2+The one-dimensional SiO of detection2/ Au nano composite material, including one-dimensional the two of sulfydryl modification
Silicon oxide and the nanometer gold that can launch fluorescence, when tested substance adds described SiO2In/Au solution, if
Tested substance contains Hg2+, the most described SiO2/ Au solution fluorescence emissive porwer reduces.Work as tested substance
In containing Hg2+Time, due to sulfydryl and Hg2+Combination can than Jin great Er cause nanometer gold reunite cause fluorescence to send out
Penetrate intensity to reduce.Due to only Hg in common ion2+Combination can be bigger than gold, therefore other ion pair detection
The impact of effect is less, shows stronger anti-ion interference ability.
A kind of for Hg2+The one-dimensional SiO of detection2/ Au nano composite material, nanometer gold and one-dimensional silicon dioxide
Between connected by sulfydryl.Due to sulfydryl and Hg2+Combination can be bigger than gold, Hg2+Capture sulfydryl and make nanometer
Gold is reunited, and shows as fluorescent emission intensity and reduces.But other ion is due to more weak than gold with the binding ability of sulfydryl
And the interference that produces is less, the most one-dimensional SiO2/ Au nano composite material is for Hg2+Have good during detection
Good selectivity.
A kind of for Hg2+The one-dimensional SiO of detection2/ Au nano composite material, as Hg in tested substance2+Dense
Degree is between 5-200nmol L-1Time, described one-dimensional SiO2/ Au Nanocomposite solution fluorescent emission intensity with
Hg2+Concentration has good linear relationship, therefore can be used for Hg2+Detection by quantitative.At Hg2+Concentration 5-200
nmol L-1Time, linear dependence standard variance is 0.999；At Hg2+Concentration 5-500nmol L-1Time, linearly
Correlation criterion variance is 0.985, and one-dimensional SiO is described2/ Au nano composite material can be used for wider concentration range
Interior Hg2+Detection by quantitative.Described one-dimensional SiO is known by calculating2/ Au nano composite material is to Hg2+Inspection
Rising limit is 4nmol L-1。
A kind of for Hg2+The one-dimensional SiO of detection2/ Au nano composite material, can be repeated for Hg2+Detection.
Due to one-dimensional SiO2/ Au nano composite material radial dimension is nanoscale, and axial dimension has reached micron order, because of
This can be saved by recycling after being centrifuged, processing while having bigger contact response area significantly
About cost, has a considerable economic worth.
Below with reference to the drawings and specific embodiments, technical scheme is further described.
Embodiment 1:
The preparation of one-dimensional SiO2/Au nano composite material
(1) preparation of one-dimensional small peptide self assembly solution
Being dissolved in the water by the amphipathic small peptide of certain mass, ultrasonic disperse, regulation is to optimum pH, room temperature
Stand, obtain one-dimensional small peptide self assembly solution；
(2) synthesis of nanometer gold
Taking mol ratio is that the glutathione solution of 1:5-1:30, chlorauric acid solution mix with ultra-pure water,
React 1-12 hour at 30-90 DEG C, obtain the nano-Au solution of glutathion protection；
(3) preparation of one-dimensional SiO2/Au nano composite material
1) in organic solvent, add hydrosulphonyl silane and the silica precursor that mol ratio is 1:2-1:20, stir
Mix uniformly, obtain silane mixture solution；
2) silane mixture solution is joined in (1) gained one-dimensional small peptide self assembly solution, mix homogeneously,
Regulation pH value of solution is to 5-9, and after reaction certain time, centrifugal, carrying out washing treatment, obtains white precipitate；
3) gained white precipitate is dispersed in water, mixes with (2) gained nano-Au solution, at 10-40 DEG C
Stirring reaction 3-8 hour, by centrifugation, washing, dried, obtain one-dimensional SiO2/ Au nano composite material.
Embodiment 2
One-dimensional SiO2The pattern of/Au nano composite material, structure and photoluminescent property characterize
High resolution transmission electron microscopy, model: JEM-2100UHR, instrument manufacturer facility man: NEC
(JEOL), accelerating potential: 200kV；
Spectrofluorophotometer, model: FluoroMax-4, instrument manufacturer facility man: France Horiba Jobin Yvon
Company produces；
Atomic absorption spectrum, model: Contr AA 700, instrument manufacturer facility man: Jena, Germany company.
The present embodiment combines high resolution transmission electron microscopy and observes one-dimensional SiO2The shape of/Au nano composite material
Looks, structure, concrete, first by sample dispersion in dehydrated alcohol, drop on the copper mesh being coated with carbon film, 5
Absorbing unnecessary liquid with filter paper after minute, drying at room temperature puts into sample room, evacuation, regulation after 1 hour
Suitably resolution and focal length, select suitable time of exposure, take pictures.
From the transmission electron microscope picture (Fig. 1) of sample it can be seen that gained sample be a diameter of 10-15 nanometer,
Length reaches the one-dimensional nano structure of the most thousands of hundreds of nanometer, in these nanostructureds, is dispersed with
The higher stain of contrast, diameter only has 1-3 nanometer.The atomic absorption spectrum of sample proves gold, shows nanometer
Gold is the most successfully anchored on silica nano fibrous.
The present embodiment uses spectrofluorophotometer to prepared one-dimensional SiO2/ Au nano composite material is carried out
Characterize, concrete, sample is disperseed in water, it is placed in the special colorimetric of fluoroscopic examination that light path is 10 millimeters
In ware, use the wavelength of 400 nanometers to excite, gather the fluorescence emission spectrum in 470-750 nanometer range.
From the fluorescence emission spectrum (Fig. 2) of sample it can be seen that one-dimensional SiO2/ Au nano composite material exists
600 nm have obvious fluorescence emission peak, and single one-dimensional silica nanometer is fine before connecting gold
Dimension does not has corresponding fluorescence emission peak in this region, proves that nanometer gold has been connected to one-dimensional two further
Silicon oxide surface, and connection procedure do not changes its photoluminescent property.
The different ions with same concentrations is joined one-dimensional SiO2In/Au Nanocomposite solution, utilize
The fluorescent spectrometry inspection different ions impact on its fluorescent emission behavior.As shown in Figure 3A, when adding Hg2+
Time, occur in that obvious Fluorescence-quenching, and the impact of other ion is the most notable.Pass through different ions
Fluorescent emission intensity value (Fig. 3 B) in 600 nanometers compares discovery, only Hg2+One can be significantly reduced
Dimension SiO2The fluorescence intensity of/Au nano composite material, shows the one-dimensional SiO invented2/ Au nano composite material
To Hg2+Detection has good anti-interference.
Embodiment 3
One-dimensional SiO2/ Au nano composite material is at Hg2+Application in detection
The different Hg of preparation2+The standard solution of concentration, with one-dimensional SiO2Use after the mixing of/Au nano composite material
Spectrofluorophotometer detects, as shown in Figure 4, along with Hg in testing sample2+The increase of concentration, its
Fluorescent emission intensity at 600 nm reduces.By fluorescent emission intensity and Hg2+Concentration is mapped, such as figure
Shown in 5A, it is shown more clearly by this rule.Especially work as Hg2+Concentration is at 5-200nmol L-1Time, its
Fluorescent emission intensity and concentration have good linear relationship, and as shown in Figure 5 B, standard variance is 0.999,
Therefore can be used for Hg2+Detection by quantitative.
By used one-dimensional SiO2/ Au nano composite material can be repeated for Hg after treatment2+Detection,
And maintain higher fluorescence recovery efficiency, as shown in Figure 6, after 5 circulate, its fluorescence recovers
Coefficient is more than 95%.
Claims (10)
1. one kind is used for Hg2+The one-dimensional SiO of detection2The preparation method of/Au nano composite material, its feature exists
In: comprise the following steps:
1) in organic solvent, add hydrosulphonyl silane and silica precursor, stir, obtain silane and mix
Close solution；
2) silane mixture solution is joined in one-dimensional small peptide self assembly solution, mix homogeneously, regulate pH value of solution
To designated value, after reaction certain time, centrifugal, carrying out washing treatment, obtains white precipitate；
3) described white precipitate is dispersed in water, mixes with nano-Au solution, stirring reaction under uniform temperature
Certain time, by centrifugation, washing, dried, obtain one-dimensional SiO2/ Au nano composite material.
The most one-dimensional SiO2The preparation method of/Au nano composite material, its feature exists
In step 1) in hydrosulphonyl silane be in mercaptopropyltriethoxysilane, mercaptopropyl trimethoxysilane at least
One, silica precursor is at least one in tetraethyl orthosilicate, methyl silicate, positive silicic acid, molten
Agent is at least one in isopropanol, ethanol, methanol, acetone.
The most one-dimensional SiO2The preparation method of/Au nano composite material, its feature exists
In: described hydrosulphonyl silane is 1:2-1:20 with the ratio of silica precursor.
One-dimensional SiO the most according to claim 12The preparation method of/Au nano composite material, its feature
It is: described one-dimensional small peptide self assembly solution is prepared by the following method:
By the small peptide (X of certain massmYnType small peptide, X is glycine, alanine, leucine, different bright ammonia
At least one in acid, Y is at least one in lysine, arginine, histidine, and m is not more than 6, n
It is not more than 2) it is dissolved in the water, ultrasonic disperse, regulate to optimum pH, room temperature stands, obtains one-dimensional short
Peptide assembles solution.
One-dimensional SiO the most according to claim 12The preparation method of/Au nano composite material, its feature
It is: nanometer gold is prepared by the following method:
Take a certain amount of glutathione solution, chlorauric acid solution, ultra-pure water mixing, glutathion and gold chloride
Mol ratio be 1:5-1:30, at 30-90 DEG C react 1-12 hour, obtain glutathion protection nanometer gold
Solution.
The most one-dimensional SiO2The preparation method of/Au nano composite material, its feature exists
In: described white precipitate is 3-8 hour with the response time of nanometer gold, reaction temperature 10-40 DEG C.
7. one kind is used for Hg2+The one-dimensional SiO of detection2/ Au nano composite material, it is characterised in that include sulfydryl
The one-dimensional silicon dioxide modified and the nanometer gold that fluorescence can be launched, described when tested substance is added
SiO2In/Au solution, if tested substance contains Hg2+, the most described SiO2/ Au solution fluorescence emissive porwer drops
Low.
The most according to claim 7 for Hg2+The one-dimensional SiO of detection2/ Au nano composite material, its
It is characterised by between nanometer gold and one-dimensional silicon dioxide being connected by sulfydryl.
The most according to claim 7 for Hg2+The one-dimensional SiO of detection2/ Au nano composite material, its
It is characterised by, works as Hg2+Concentration is between 5-200nmol L-1Time, described one-dimensional SiO2/ Au nano composite material
Solution fluorescence emissive porwer and Hg2+Concentration has good linear relationship, therefore can be used for Hg2+Quantitative inspection
Survey.
The most according to claim 7 for Hg2+The one-dimensional SiO of detection2/ Au nano composite material,
It is characterized in that: described one-dimensional SiO2/ Au nano composite material can be repeated for Hg2+Detection.
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