CN106544012A - High selectivity determines the water soluble fluorescence nano silicon particles synthesis of trace TNP and applies - Google Patents
High selectivity determines the water soluble fluorescence nano silicon particles synthesis of trace TNP and applies Download PDFInfo
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- CN106544012A CN106544012A CN201610964476.6A CN201610964476A CN106544012A CN 106544012 A CN106544012 A CN 106544012A CN 201610964476 A CN201610964476 A CN 201610964476A CN 106544012 A CN106544012 A CN 106544012A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 title description 7
- 238000003786 synthesis reaction Methods 0.000 title description 7
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000001514 detection method Methods 0.000 claims abstract description 19
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 14
- 239000002360 explosive Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 8
- 230000014759 maintenance of location Effects 0.000 claims description 7
- 229950000845 politef Drugs 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 7
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical class OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 abstract description 53
- 230000000007 visual effect Effects 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 239000011856 silicon-based particle Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 37
- 238000012360 testing method Methods 0.000 description 8
- 150000005206 1,2-dihydroxybenzenes Chemical class 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 238000000502 dialysis Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- DYSXLQBUUOPLBB-UHFFFAOYSA-N 2,3-dinitrotoluene Chemical compound CC1=CC=CC([N+]([O-])=O)=C1[N+]([O-])=O DYSXLQBUUOPLBB-UHFFFAOYSA-N 0.000 description 4
- 239000007853 buffer solution Substances 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000015784 hyperosmotic salinity response Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 3
- 231100000716 Acceptable daily intake Toxicity 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000012921 fluorescence analysis Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- SPSSULHKWOKEEL-UHFFFAOYSA-N 2,4,6-trinitrotoluene Chemical class CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O SPSSULHKWOKEEL-UHFFFAOYSA-N 0.000 description 1
- OVOJUAKDTOOXRF-UHFFFAOYSA-N 2,4-dinitrobenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O OVOJUAKDTOOXRF-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 208000007502 anemia Diseases 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 125000006575 electron-withdrawing group Chemical group 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000003018 immunoassay Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000001871 ion mobility spectroscopy Methods 0.000 description 1
- 230000003908 liver function Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 125000005245 nitryl group Chemical group [N+](=O)([O-])* 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical compound C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 1
- -1 pyrotechnics Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000002760 rocket fuel Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical compound [Al+3].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 TVIVIEFSHFOWTE-UHFFFAOYSA-K 0.000 description 1
- 229950002929 trinitrophenol Drugs 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888
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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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- 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"
- G01N2021/6432—Quenching
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Abstract
The invention discloses a kind of water soluble fluorescence nano silicon particles (SiNPs) with one kettle way preparation high sensitivity and high selectivity in water phase determine the new method of 2,4,6 trinitrophenols (TNP).At optimum conditions, the range of linearity that the method determines TNP is 0.02 120mg/L, and linear equation is that detection is limited to 6.7 μ g/L.On this basis, it is prepared for can be used for the reagent paper of Visual retrieval TNP.
Description
Technical field
The invention belongs to chemical field, and in particular to a kind of water solublity of detection 2，4，6-trinitrophenol (TNP)
The synthetic method of fluorescent nano particle and its application.
Background technology
TNP, also known as picric acid (PA), are a kind of nitryl aromatic explosives with strong electron-withdrawing group, and its brisance is big
In 2,4,6- trinitrotoluenes (TNT).TNP is widely used in dye industry, rocket fuel, pyrotechnics, medicine and laboratory.
Its permissible value in drinking water is 0.5mg/L, and acceptable daily intake (ADI) is 1-37 μ g/ (kg per day).Therefore,
In a large number can severe contamination soil and surface water using TNP.When people suction, swallow or in a large number contact TNP when can cause skin mistake
The symptom such as quick, anemia, cancer, abnormal liver function and respiratory system be impaired.In view of TNP is to the severe contamination of environment and to the mankind
The threat of health, sensitive and selective enumeration method TNP have caused the extensive concern of people.Additionally, nitryl aromatic explosive is such as
Dinitrotoluene (DNT) (DNT), Nitrobenzol (NB) and TNT have interference to detecting TNP.As TNP and TNT have very strong electricity
Sub- affinity, TNT are particularly evident to the interference for detecting TNP.So, in the mixture of nitryl aromatic explosive detect TNP into
For a challenging task.So far, detect that the method for nitryl aromatic explosive mainly has surface-enhanced Raman light
Spectrum, high performance liquid chromatography, dynamic light scattering, solid-phase microextraction-ion mobility spectrometry, electrochemistry and enzyme immunoassay.But on
There are some shortcomings in the method for stating, such as high cost, instrumentation be complicated, extraction process length and cannot be distinguished by TNP and TNT, these
Shortcoming limits their extensive application.In contrast, fluorescence analysis method with its high sensitivity, high selectivity, it is simple to operate,
The advantages of real-time detection, low cost and portability cause the extensive concern of people and establish it is a series of detection nitryl aromatics it is quick-fried
The fluorescence analysis method of fried thing, such as ZnS:Mn2+@allyl sulfhydrate nano-complex methods, 8-hydroxyquinoline aluminum Nano microsphere method,
Graphene carbonitride (g-C3N4) method, metal organic frame (MOF) method based on Cd (II) and nitrogen-doped carbon point method etc..But
Above method has nano material synthesis when TNP is detected, and to need multistep reaction, material to prepare time-consuming, toxicity high and using having
Machine solvent etc., these shortcomings limit the extensive application of these materials.Simultaneously for various public places safe examination system and
Speech, for whether a difficult problem is remained containing TNP in suspicious item, it is difficult to there is direct method quickly to check.Therefore, develop one
The method for planting simple, harmless, highly sensitive and selective detection aqueous solution TNP is very necessary.
The content of the invention
It is an object of the invention to：
Set up the simple, synthesis that saves time with toxicity is low, have good stability, the excellent water solublity SiNPs new methods of optical property；
Synthesis detects the fluorescence SiNPs of TNP in water phase；On this basis, detection is set up using the excellent properties of fluorescence SiNPs
TNP fluorescence new method simultaneously prepares the fluorescence SiNPs reagent paper for detecting TNP.
The present invention is realized by following steps：
(1) synthesis of SiNPs
A, add deionized water in round-bottomed flask, DAMO is added in whipping process, catechol is subsequently added, fully
Stirring.
B, said mixture solution is transferred in politef autoclave, when 200 DEG C, reacts 4h, natural cooling
To room temperature.
C, dialyse in the bag filter of 1000Da (molecular weight cutoff) 6h by the SiNPs solution for preparing.
D, by the SiNPs solution storages dialysed in 4 DEG C of refrigerator for detection below.
Further, N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes with catechol mol ratio are：9.3:100.
(2) structure of SiNPs is characterized with methods such as XPS, FT-IR.
(3) fluorescence intensity when heat stability to SiNPs, anti-light Bleachability, salt tolerance and different pH value is examined
Examine.Determine condition determination, set up the method that TNP is determined in water phase, the fluorescence SiNPs reagent paper for preparing detection TNP.
(4) in aqueous solution TNP measure
A SiNPs solution PBS (pH=7.4) buffer solution for preparing is diluted 1000 times by ()；In SiNPs weak solutions
The middle TNP solution for adding variable concentrations, places 1min；It is 430nm in excitation wavelength, fluorescence is surveyed when launch wavelength is 512nm strong
Degree；The slit width of excitation wavelength and launch wavelength is 5nm.
B () SiNPs is determined as follows to the selectivity of TNP：Finite concentration is added in 3mL SiNPs weak solutions
Inorganic ionic solution or nitryl aromatic explosive solution；According to the parametric measurement fluorescence intensity of setting in (a).All experiments are equal
Carry out at ambient temperature.
(5) preparation of fluorescent test paper strip and the Visual retrieval to TNP
A quantitative filter paper is immersed in and is diluted in 2.5 times of SiNPs solution with PBS (pH=7.4) buffer solution by ()；Immersion
After 20min, filter paper from solution is pipetted out be placed in 50 DEG C of baking oven be dried；After filter paper naturally cools to room temperature, will
Filter paper is cut into reagent paper.
B () instills the TNP solution of 10 μ L variable concentrations in the test strips for preparing, after solvent natural evaporation, will examination
Paper slip is placed in the color change of observation filter paper bar under the uviol lamp of 365nm and determines that TNP whether there is.Above-mentioned experiment is at room temperature
Carry out.
Benefit of the invention is that:
This preparation method is simple to operate, save time, and prepared SiNPs has good heat stability, stronger salt tolerance
With excellent anti-light bleaching power；The method choice for determining TNP in water sample set up is good, and sensitivity is high；The fluorescence of preparation
Reagent paper can be used for the Visual retrieval of TNP.In the present invention, it is utilized respectively N- (2- aminoethyls) -3- aminopropyl trimethoxy silicon
Alkane (DAMO) and catechol are that silicon source and reducing agent have synthesized water miscible fluorescence SiNPs.Compared with existing method, the party
Method avoids multistep and time-consuming material preparation process.SiNPs prepared by the method has good heat stability, and excellent is anti-
Photobleaching ability and salt tolerance, quantum yield are 7.1%.The fluorescence of SiNPs is quenched after TNP is added, and which is quenched mechanism and is
Interior filtering effect (IFE).On this basis, the present invention establishes a kind of highly sensitive in water phase and high selectivity and detects TNP's
New method.Also it is prepared for a kind of fluorescence SiNPs reagent paper of detection TNP simultaneously.
Description of the drawings
The infrared spectrogram of Fig. 1 SiNPs.
The x-ray photoelectron energy spectrum diagram of Fig. 2 SiNPs.
Impact of Fig. 3 temperature to SiNPs normalization fluorescence intensities.
The impact of Fig. 4 inorganic ionss (A) and nitryl aromatic explosive (B) to detection TNP.
Impact of Fig. 5 (a) TNP concentration to SiNPs reagent paper fluorescence intensities；B () other nitryl aromatic explosive mixture are dense
Impact of the degree to SiNPs reagent paper fluorescence intensities；C () TNP and other nitryl aromatic explosive mixture concentrations are glimmering to SiNPs reagent paper
The impact of light intensity；Concentration is from left to right followed successively by 0,0.01,0.05,0.1,0.5,1.0mg/mL.
The measurement result of TNP in Fig. 6 nitryl aromatic explosives.The concentration of TNP is 1mg/L；Nitryl aromatic explosive DNB,
The concentration of DNBA, DNT, NB, NT and TNT is 5mg/L (in figure, NAE represents nitryl aromatic explosive mixture).
Specific embodiment
Embodiment 1
50mL deionized waters are added in 100mL round-bottomed flasks, 5mL DAMO is added in whipping process, is subsequently added
25mg catechols, after being sufficiently stirred for 1min, said mixture solution are transferred in politef autoclave, 200
DEG C when react 4h, naturally cool to room temperature.Then by the SiNPs solution for preparing 1000Da (molecular weight cutoff) bag filter
Middle dialysis 6h.Finally, by the SiNPs solution storages dialysed in 4 DEG C of refrigerator for detection below.N- (2- ammonia second
Base) -3- aminopropyl trimethoxysilanes with catechol optimum molar ratio are：9.3:100.
Embodiment 2
50mL deionized waters are added in 100mL round-bottomed flasks, 2mL DAMO is added in whipping process, is subsequently added
11mg catechols, after being sufficiently stirred for 1min, said mixture solution are transferred in politef autoclave, 200
DEG C when react 4h, naturally cool to room temperature.Then by the SiNPs solution for preparing 1000Da (molecular weight cutoff) bag filter
Middle dialysis 6h.Finally, by the SiNPs solution storages dialysed in 4 DEG C of refrigerator for detection below.
Embodiment 3
30mL deionized waters are added in 50mL round-bottomed flasks, 5mL DAMO is added in whipping process, is subsequently added
20mg catechols, after being sufficiently stirred for 1min, said mixture solution are transferred in politef autoclave, 200
DEG C when react 4h, naturally cool to room temperature.Then by the SiNPs solution for preparing 1000Da (molecular weight cutoff) bag filter
Middle dialysis 6h.Finally, by the SiNPs solution storages dialysed in 4 DEG C of refrigerator for detection below.
Embodiment 4
10mL deionized waters are added in 25mL round-bottomed flasks, 5mL DAMO is added in whipping process, is subsequently added
20mg catechols, after being sufficiently stirred for 1min, said mixture solution are transferred in politef autoclave, 200
DEG C when react 4h, naturally cool to room temperature.Then by the SiNPs solution for preparing 1000Da (molecular weight cutoff) bag filter
Middle dialysis 6h.Finally, by the SiNPs solution storages dialysed in 4 DEG C of refrigerator for detection below.
Embodiment 5
(1) synthesis of SiNPs
10mL deionized waters are added in 25mL round-bottomed flasks, 2mL DAMO is added in whipping process, is subsequently added
11mg catechols, after being sufficiently stirred for 1min, said mixture solution are transferred in politef autoclave, 200
DEG C when react 4h, naturally cool to room temperature.Then by the SiNPs solution for preparing 1000Da (molecular weight cutoff) bag filter
Middle dialysis 6h.Finally, by the SiNPs solution storages dialysed in 4 DEG C of refrigerator for detection below.
(2) structure of SiNPs is characterized with methods such as XPS, FT-IR.
(3) fluorescence intensity when heat stability to SiNPs, anti-light Bleachability, salt tolerance and different pH value is examined
Examine.Determine condition determination, set up the method that TNP is determined in water phase, the fluorescence SiNPs reagent paper for preparing detection TNP.
(4) in water phase TNP measure
A SiNPs solution 10mM PBS (pH=7.4) buffer solution for preparing is diluted 1000 times by ()；In 3.0mL
The TNP solution of variable concentrations is added in SiNPs weak solutions, 1min is placed；It is 430nm in excitation wavelength, launch wavelength is 512nm
When survey fluorescence intensity；The slit width of excitation wavelength and launch wavelength is 5nm.
B () SiNPs is determined as follows to the selectivity of TNP：Finite concentration is added in 3mL SiNPs weak solutions
Inorganic ionic solution or nitryl aromatic explosive solution；According to the parametric measurement fluorescence intensity of setting in (a).All experiments are equal
Carry out at ambient temperature.
(5) preparation of fluorescent test paper strip and the Visual retrieval to TNP
A quantitative filter paper is immersed in and is diluted in 2.5 times of SiNPs solution with 10mM PBS (pH=7.4) buffer solution by ()；
After immersion 20min, filter paper is pipetted out to be placed in 50 DEG C of baking oven from solution it is dried 20min；Treat that filter paper is naturally cooled to
After room temperature, filter paper is cut into into test strips.
B () instills the TNP solution of 10 μ L variable concentrations in the test strips for preparing, after solvent natural evaporation, will examination
Paper slip is placed in the color change of observation filter paper bar under the uviol lamp of 365nm and determines that TNP whether there is.Above-mentioned experiment is at room temperature
Carry out.
The measurement result of TNP in 1 water sample of table
Fluorescent nano particle synthesized by the present invention be can be seen that from Fig. 4,5 has fabulous selectivity, for various interference
Thing performance is excellent, can use as environmental testing and safety check test.
Embodiment 6
Detection mode when safety check is tested
TNP is yellow powdery solid, similar to other nitro explosive outward appearance, with extremely strong explosivity.On airport
Or during other public arenas discovery suspicious items, can be tested by the reagent paper mentioned in embodiment 5, in the examination for preparing
10 μ L suspicious item solution are instilled on paper slip, after solvent natural evaporation, test strips is placed under the uviol lamp of 365nm and is observed filter paper
The color change of bar determines that TNP whether there is.If there is the fluorescence intensity change shown in Fig. 5, then illustrate there is pole in suspicious item
Big probability is mixed with TNP, should process in time, it is to avoid dangerous.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, should all be included within the scope of the present invention.
Claims (5)
1. a kind of water soluble fluorescence nano silicon particles of measure trace TNP, it is characterised in that using N- (2- aminoethyls) -3- ammonia
Propyl trimethoxy silicane (DAMO) synthesizes the water soluble fluorescence nano silicon particles for reducing agent as silicon source, catechol.
2. a kind of water soluble fluorescence nano silicon particles of measure trace TNP according to claim 1, it is characterised in that system
Preparation Method is：
A, add deionized water in round-bottomed flask, DAMO is added in whipping process, catechol is subsequently added, is fully stirred
Mix.
B, said mixture solution is transferred in politef autoclave, 4h is reacted when 200 DEG C, naturally cool to room
Temperature.
C, dialyse in the bag filter of 1000Da 6h by the SiNPs solution for preparing.
D, by the SiNPs solution storages dialysed in 4 DEG C of refrigerator for detection below.
3. the water soluble fluorescence nano silicon particles preparation method of a kind of measure trace TNP according to claim 2, its feature
It is that N- (2- aminoethyls) -3- aminopropyl trimethoxysilanes are with catechol mol ratio：9.3:100.
4. the water soluble fluorescence nano silicon particles preparation method of a kind of measure trace TNP according to claim 2, its feature
It is that the method can be used to make reagent paper or reagent, when preparing reagent paper, quantitative filter paper is immersed in and is buffered with the PBS of pH=7.4
Solution is diluted in 2.5 times of SiNPs solution；After immersion 20min, filter paper from solution is pipetted out it is placed in 50 DEG C of baking oven
It is dried 20min；After filter paper naturally cools to room temperature, filter paper is cut into into reagent paper.
5. the water soluble fluorescence nano silicon particles reagent paper of a kind of measure trace TNP according to claim 4, its feature exist
In can be used for the detection of TNP in trace explosive and the detection of trace TNP in water sample.
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