CN109142295A - A method of Norfloxacin is identified using sulphur quantum dots characterization cobalt ions and relay - Google Patents
A method of Norfloxacin is identified using sulphur quantum dots characterization cobalt ions and relay Download PDFInfo
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- CN109142295A CN109142295A CN201810879354.6A CN201810879354A CN109142295A CN 109142295 A CN109142295 A CN 109142295A CN 201810879354 A CN201810879354 A CN 201810879354A CN 109142295 A CN109142295 A CN 109142295A
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical class [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 109
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 229910001429 cobalt ion Inorganic materials 0.000 title claims abstract description 99
- OGJPXUAPXNRGGI-UHFFFAOYSA-N norfloxacin Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNCC1 OGJPXUAPXNRGGI-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229960001180 norfloxacin Drugs 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000012512 characterization method Methods 0.000 title claims abstract description 16
- 239000005864 Sulphur Substances 0.000 claims abstract description 93
- 239000002096 quantum dot Substances 0.000 claims abstract description 93
- 239000000243 solution Substances 0.000 claims abstract description 93
- 239000012488 sample solution Substances 0.000 claims abstract description 45
- 238000002189 fluorescence spectrum Methods 0.000 claims abstract description 34
- 230000005284 excitation Effects 0.000 claims abstract description 25
- 238000001514 detection method Methods 0.000 claims abstract description 24
- 238000000295 emission spectrum Methods 0.000 claims abstract description 22
- 239000012490 blank solution Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012153 distilled water Substances 0.000 claims abstract description 15
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 11
- 229910001424 calcium ion Inorganic materials 0.000 claims description 11
- 229910017052 cobalt Inorganic materials 0.000 claims description 8
- 239000010941 cobalt Substances 0.000 claims description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 description 15
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 8
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 8
- 230000035945 sensitivity Effects 0.000 description 7
- 238000000862 absorption spectrum Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000008280 blood Substances 0.000 description 5
- 210000004369 blood Anatomy 0.000 description 5
- 150000001768 cations Chemical class 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000000171 quenching effect Effects 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 description 2
- 230000004087 circulation Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 description 2
- -1 plumbi nitras Chemical compound 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 206010016654 Fibrosis Diseases 0.000 description 1
- UIOFUWFRIANQPC-JKIFEVAISA-N Floxacillin Chemical compound N([C@@H]1C(N2[C@H](C(C)(C)S[C@@H]21)C(O)=O)=O)C(=O)C1=C(C)ON=C1C1=C(F)C=CC=C1Cl UIOFUWFRIANQPC-JKIFEVAISA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- 206010003549 asthenia Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 230000000747 cardiac effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004761 fibrosis Effects 0.000 description 1
- 229960004273 floxacillin Drugs 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
Classifications
-
- 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"
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Optics & Photonics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The present invention provides a kind of method using sulphur quantum dots characterization cobalt ions and relay identification Norfloxacin, the method using sulphur quantum dots characterization cobalt ions includes: that the sulphur quantum dot of the first mass parts is dissolved in distilled water respectively, forms blank solution；The sulphur quantum dot of second mass parts is dissolved in solution to be measured, sample solution is formed；Further include: the blank solution is scanned under 360nm excitation wavelength by sepectrophotofluorometer, the blank fluorescence emission spectrum within the scope of 380nm~450nm；The sample solution is scanned under 360nm excitation wavelength by sepectrophotofluorometer, the fluorescent emission spectrum within the scope of 380nm~450nm；When the fluorescent emission spectrum wave crest does not occur within the scope of 395nm~415nm, determines in the solution to be measured and contain cobalt ions；Wherein, the wave crest appears within the scope of 395nm~415nm of the blank fluorescence emission spectrum.This programme can be shortened the detection duration of cobalt ions.
Description
Technical field
The present invention relates to technical field of chemistry, in particular to a kind of to identify promise using sulphur quantum dots characterization cobalt ions and relay
The method of Flucloxacillin.
Background technique
Cobalt is one of microelement necessary to growth in humans develops, and has close ties with human health, long-term to lack
Weary cobalt can cause surra, but excess intake can also be done harm to huamn body.Cobalt in water environment is exceeded, can generate many
To human body detrimental effect, such as lead to interstitial fibrosis or cardiac asthenia etc..Therefore, in environment measuring, cobalt is listed in weight
One of detection project wanted.
Currently, the detection method of cobalt ions is mainly chemoluminescence method, spectrophotometry and atomic absorption spectrography (AAS) etc..It adopts
When detecting cobalt ions with these methods, it is both needed to carry out pre-treatment to sample to be tested, for example, it is desired to sample to be tested
In interfering ion sheltered or separated, this causes the detection of cobalt ions to take a long time.
Summary of the invention
The embodiment of the invention provides it is a kind of using sulphur quantum dots characterization cobalt ions and relay identification Norfloxacin method,
It can be shortened detection duration.
In a first aspect, the embodiment of the invention provides a kind of methods using sulphur quantum dots characterization cobalt ions, comprising:
The sulphur quantum dot of the first mass parts is dissolved in distilled water respectively, forms blank solution；
The sulphur quantum dot of second mass parts is dissolved in solution to be measured, sample solution is formed；
Further include:
The blank solution is scanned under 360nm excitation wavelength by sepectrophotofluorometer, in 380nm~450nm model
Enclose interior blank fluorescence emission spectrum；
The sample solution is scanned under 360nm excitation wavelength by sepectrophotofluorometer, in 380nm~450nm model
Enclose interior fluorescent emission spectrum；
When the fluorescent emission spectrum wave crest does not occur within the scope of 395nm~415nm, determine described to be measured molten
Contain cobalt ions in liquid；Wherein, the wave crest appears within the scope of 395nm~415nm of the blank fluorescence emission spectrum.
The result shows that, the blank fluorescence emission spectrum of blank solution occurs most within the scope of 395nm~415nm after testing
There is wave crest in big absorbing wavelength, and the fluorescent emission spectrum of the sample solution containing cobalt ions is in 395nm~415nm
Fluorescence intensity in range is much smaller than the fluorescence intensity of blank fluorescence emission spectrum in the range, and blank fluorescence emission spectrum is former
Some wave crests disappear, and illustrate that the fluorescence intensity of sulphur quantum dot can be influenced by cobalt ions, cobalt ions has quenching effect to sulphur quantum dot.
In addition, by further detection test discovery, Na+、Fe3+、Cu2+、Mg2+、Zn2+、Pb2+、Cd2+、NH4 +、Ag+、Ni2+And Bi3+'s
Also there is wave crest within the scope of 395nm~415nm in the fluorescence emission spectrum of aqueous solution, illustrates that these cations will not be to sulfur content
Point fluorescence intensity produce bigger effect, thus illustrate sulphur quantum dot to cobalt ions have feature sensitivities, can be used for cobalt from
The detection of son.
Preferably,
It is described the sulphur quantum dot of second mass parts is dissolved in solution to be measured before, further comprise: adjust
The pH of the solution to be measured is 7~8.
Preferably,
Containing after cobalt ions in the determination solution to be measured, further comprise:
The fluorescence intensity of the sample solution and blank solution under 360nm excitation wavelength is detected respectively；
According to the following formula, the concentration of cobalt ions in the solution to be measured is calculated；
F0/F1=5.73194+9325C1
Wherein, F1Characterize fluorescence intensity of the sample solution at 360nm, F0The blank solution is characterized at 360nm
Fluorescence intensity, C1Characterize the concentration of cobalt ions in the solution to be measured.
Preferably,
The sulphur quantum dot of second mass parts is dissolved in solution to be measured described, is formed before sample solution, into
One step includes:
It detects with the presence or absence of calcium ion in the solution to be measured, if so, being carried out to the calcium ion in the solution to be measured
Separation.
Preferably,
When the volume of the distilled water is equal with the volume of the solution to be measured, first mass parts and described second
Mass parts are equal.
Second aspect, the embodiment of the invention provides a kind of method using sulphur quantum dot relay identification Norfloxacin, packets
It includes:
When the method provided using any of the above-described embodiment of the present invention determine fluorescent emission spectrum 395nm~
When not occurring wave crest within the scope of 415nm, further includes:
Target solution is added into sample solution；
The sample solution after the target solution is added by sepectrophotofluorometer scanning is in 360nm excitation wavelength
Under, the target fluorescent emission spectrum within the scope of 380nm~450nm；
When the fluorescence intensity in the target fluorescent emission spectrum is greater than corresponding wavelength in the fluorescent emission spectrum
Under fluorescence intensity when, determine and contain Norfloxacin in the target solution, and restore the sulphur quantum dot in the sample solution
To the detection activity of cobalt ions.
Preferably,
Containing after Norfloxacin in the determination target solution, further comprise:
Fluorescence intensity of the sample solution under 360nm excitation wavelength after the detection addition target solution；
According to following calculation formula, the concentration of the Norfloxacin solution is calculated；
F2=359.79632+2.85108 × 10-6C2
Wherein, F2Fluorescence intensity of the sample solution under 360nm excitation wavelength after the characterization addition target solution, C2
Characterize the concentration of the Norfloxacin solution.
Preferably,
After there is not wave crest within the scope of 395nm~415nm in the determining fluorescent emission spectrum, it is described to
It is added before target solution in the sample solution, further comprises:
According to preset period of time, fluorescence intensity of the sample solution under 360nm excitation wavelength is detected；
Determine the strength difference between the corresponding fluorescence intensity of each time cycle；
When the strength difference is less than preset threshold, execution is described to be added target solution into the sample solution.
The embodiment of the invention provides it is a kind of using sulphur quantum dots characterization cobalt ions and relay identification Norfloxacin method,
There is maximum absorption wavelength within the scope of 395nm~415nm in the blank fluorescence emission spectrum of blank solution, that is, wave crest occurs, and
Fluorescence intensity of the fluorescent emission spectrum of sample solution containing cobalt ions within the scope of 395nm~415nm is much smaller than sky
The fluorescence intensity of white fluorescence emission spectrum in the range, the original wave crest of blank fluorescence emission spectrum disappear, and illustrate sulfur content
The fluorescence intensity of point can be influenced by cobalt ions, and cobalt ions has quenching effect to sulphur quantum dot.In addition, by further detection test
It was found that Na+、Fe3+、Cu2+、Mg2+、Zn2+、Pb2+、Cd2+、NH4 +、Ag+、Ni2+And Bi3+The fluorescence emission spectrum of aqueous solution exist
Also occur wave crest within the scope of 395nm~415nm, illustrate that these cations will not generate larger shadow to the fluorescence intensity of sulphur quantum dot
It rings, to illustrate that sulphur quantum dot has feature sensitivities to cobalt ions, the detection of cobalt ions can be used for.It as a result, can be directly sharp
The cobalt ions in solution to be measured is detected with sulphur quantum dot, without being sheltered to other cations in solution to be measured
Or separation, so as to shorten the detection duration of cobalt ions.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is the different cationic solutions corresponding fluorescent emission provided by one embodiment of the present invention containing sulphur quantum dot
Spectrogram；
Fig. 2 is the fluorescence spectra of the different concentration of cobalt ions provided by one embodiment of the present invention containing sulphur quantum dot；
Fig. 3 is concentration of cobalt ions provided by one embodiment of the present invention-fluorescence intensity linear relation figure；
Fig. 4 is uv absorption spectra provided by one embodiment of the present invention；
Fig. 5 is the fluorescence spectra of the sulphur quantum dot under different pH condition provided by one embodiment of the present invention；
Fig. 6 is the fluorescence of the different cationic solutions provided by one embodiment of the present invention containing sulphur quantum dot and cobalt ions
Intensity map；
Fig. 7 is the fluorescence of the different cationic solutions provided by one embodiment of the present invention containing sulphur quantum dot and cobalt ions
Spectrogram；
Fig. 8 is invertibity testing result schematic diagram provided by one embodiment of the present invention；
Fig. 9 is the Norfloxacin of the various concentration provided by one embodiment of the present invention containing sulphur quantum dot and cobalt ions
Fluorescence spectra；
Figure 10 is blood concentration norfloxacin provided by one embodiment of the present invention-fluorescence intensity linear relation figure.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments, based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
Experimental method used in following embodiments is conventional method unless otherwise specified.In following embodiments, institute
Various kinds of equipment, reagent and the material used is that conventional commercial can obtain unless otherwise noted.
Embodiment 1: the feature sensing substance of measurement sulphur quantum dot
It is scanned by the fluorescence emission spectrum to the different sample solutions dissolved with sulphur quantum dot, determines sulphur quantum dot
Feature sense ion, specific step is as follows when measurement:
Step A1: be respectively configured concentration be the copper nitrate of 0.001mol/L, magnesium nitrate, zinc sulfate, plumbi nitras, sodium nitrate,
Each 100mL of ammonium chloride, cobalt nitrate, silver nitrate, cadmium nitrate, nickel nitrate, ferric sulfate, bismuth nitrate solution is as solution to be measured.
For each solution to be measured configured, step B1 and step C1 is executed；It is every to have detected a kind of solution to be measured, it uses
Distilled water cleans cuvette 5 times；
Step B1: taking a cuvette that the sulphur quantum dot of 2mL distilled water and 50 μ L is added, and blank solution is made.It is flat to system
Scan its corresponding blank fluorescence emission spectrum when weighing apparatus, excitation wavelength when scanning is set as 360nm, the initial value of launch wavelength
For 380nm, stop value 450nm.
Step C1: 50 μ L solution to be measured being added with microsyringe into the blank solution of step B1, form sample solution.
The corresponding fluorescent emission spectrum of the sample solution is scanned when system balance, excitation wavelength when scanning is set as 360nm,
The initial value of launch wavelength is 380nm, stop value 450nm.
The scanning result of embodiment 1 is as shown in Figure 1, from figure 1 it appears that under equal conditions to scan each sample molten
The emission spectrum of liquid, in addition to the sample solution made from the cobalt nitrate solution, other cations (Na+、Fe3+、Cu2+、Mg2+、Zn2+、Pb2 +、Cd2+、NH4 +、Ag+、Ni2+And Bi3+) maximum absorption wavelength occurs within the scope of wavelength 395nm~415nm in sample solution, it is various
In solion only have the corresponding fluorescent emission spectrum of cobalt ions solution compared to blank fluorescence emission spectrum variation most
Obviously, its fluorescence intensity within the scope of 395nm~415nm exists far from other ions, and much smaller than blank fluorescence emission spectrum
Fluorescence intensity within the scope of this, therefore illustrate that cobalt ions has quenching effect to sulphur quantum dot.This may be because of cobalt ions and sulphur
The surface group of quantum dot is acted on, so that the charge of sulphur quantum dot surface is shifted, cobalt ions and sulphur quantum dot
Between have occurred aggregation inducing effect, and the transfer of sulphur quantum dot surface charge is so that the fluorescence intensity of sulphur quantum dot declines, from
And there is quenching effect.
Embodiment 2
By measuring influence of the cobalt ions solution of various concentration to sulphur quantum dot fluorescence intensity, sulfur content is further determined that
Sensing of the point to cobalt ions.
Embodiment 2 may comprise steps of:
Step A2: taking a cuvette that the sulphur quantum dot of 2mL distilled water and 50 μ L is added, and blank solution is made.It is flat to system
Scan its corresponding blank fluorescence emission spectrum when weighing apparatus, excitation wavelength when scanning is set as 360nm, the initial value of launch wavelength
For 380nm, stop value 450nm.
In following steps, excitation wavelength is disposed as 360nm, and the initial value of launch wavelength is disposed as 380nm, transmitted wave
Long stop value is disposed as 450nm.
Step B2: it is 0.001mol/L's that 20 μ L concentration are added into blank solution made from step A2 with microsyringe
Cobalt nitrate solution measures the fluorescence emission spectrum of the sample solution under equal conditions.Then it is molten gradually to increase by 20 μ L cobalt nitrates
Liquid measures its fluorescence emission spectrum, until fluorescence emission spectrum is no longer with the increase of concentration of cobalt ions in sample solution and
Variation.
The measurement result of embodiment 2 is as shown in Figure 2, wherein Fig. 2 indicates 1 to 11 corresponding concentration of cobalt ions (mol/L)
Successively are as follows: 0,10-5, 2 × 10-5, 3 × 10-5, 4 × 10-5, 5 × 10-5, 6 × 10-5, 7 × 10-5, 8 × 10-5, 9 × 10-5, i.e., 1 pair
The concentration of cobalt ions answered is 0, the blank fluorescence emission spectrum that as step A2 is obtained.Figure it is seen that as cobalt ions is dense
Degree increases, and the fluorescence intensity of sulphur quantum dot gradually decreases, this also illustrates sulphur quantum dot to the sensitivities of cobalt ions.
By further to the fluorescence at 410nm in the corresponding fluorescence emission spectrum of the cobalt nitrate solution of various concentration
The analysis of intensity can obtain concentration of cobalt ions-fluorescence intensity relational graph as shown in Figure 3.As can be seen from Figure 3 concentration of cobalt ions
There are linear relationships between the fluorescence intensity of sulphur quantum dot: F0/F1=5.73194+9325C1, R=0.96102, by linearly closing
System can also illustrate, as concentration of cobalt ions increases, the fluorescence intensity of sulphur quantum dot is reduced.Also, due to concentration of cobalt ions and sulphur
There are good linear relationships between the fluorescence intensity of quantum dot, then when using sulphur quantum dots characterization concentration of cobalt ions, can lead to
The fluorescence intensity of measurement sample solution is crossed, above-mentioned linear equation is then utilized, solves the concentration of cobalt ions in solution to be measured.By
This can quickly and easily test out the concentration of cobalt ions in solution to be measured.Experimental result surface, sulphur quantum dot can be in 0~9 × 10-
Cobalt ions is accurately detected within the scope of 5mol/L.
In addition, to cobalt nitrate solution and containing cobalt ions respectively using UV-3100PC type ultraviolet-uisible spectrophotometer
Sample solution carries out ultra-violet absorption spectrum measurement.When measurement, reference is done with distilled water, ultraviolet suction is carried out to 200~800nm of wavelength
Spectral scan is received, measurement result is as shown in Figure 4.The a indicated in Fig. 4 corresponds to the ultra-violet absorption spectrum of cobalt nitrate solution, Fig. 4 acceptance of the bid
The ultra-violet absorption spectrum of the corresponding sample solution containing cobalt ions of the b shown.Figure 4, it is seen that two ultraviolet spectras have
Apparent difference, this also illustrates ultra-violet absorption spectrum of the sulphur quantum dot to cobalt ions to have a significant effect, it changes cobalt ions
Ultra-violet absorption spectrum, to illustrate sulphur quantum dot to the sensitivities of cobalt ions.
Embodiment 4: the detection to fluorescence property of the sulphur quantum dot under different acid or alkali environments
The sulphur quantum dot of 2mL distilled water and 50 μ L is added in cuvette, it is corresponding in pH3~10 to measure it respectively
Fluorescence spectrum, to determine fluorescence property of the sulphur quantum dot under different acid or alkali environments, measurement result is as shown in Figure 5.It can from Fig. 5
To find out, the fluorescence intensity highest of sulphur quantum dot when pH=7, and the fluorescence intensity of sulphur quantum dot is most weak when pH=10, and in pH
The fluorescence intensity of sulphur quantum dot is weaker when=9.Therefore, when using sulphur quantum dot, the pH of solution to be measured can be adjusted to 7
~8, so that sulphur quantum dot will not drastically reduce the fluorescence intensity of itself because of environmental pH, to be conducive to in solution to be measured
Sense the Accurate Determining of ion.
Embodiment 5: the interfering ion during sulphur quantum dots characterization cobalt ions is determined
Embodiment 5 may comprise steps of:
Step A5: respectively compound concentration be the calcium chloride of 0.001mol/L, magnesium nitrate, zinc sulfate, plumbi nitras, sodium nitrate,
Chromic nitrate, cadmium nitrate, ammonium chloride, zinc nitrate, copper nitrate solution.
For each solution configured, execute step B5, and it is every detected a kind of solution, compare wash with distilled water
Color ware 5 times；
Step B5: 2mL distilled water, the sulphur quantum dot of 50 μ L and 20 μ L cobalt nitrate solutions in cuvette, then to cuvette
A kind of solution that 20 μ L step A5 of middle addition make.Measurement is 360nm in excitation wavelength when system balance, and launch wavelength is
The fluorescence intensity of 410nm.
The scanning result of embodiment 5 is as shown in fig. 6, from fig. 6 it can be seen that most metal ions are almost to cobalt ions
The noiseless effect of detection, but calcium ion is affected, and has been more than the influence that other metal ions detect cobalt ions.Cause
This can first be detected in solution to be measured when being detected using sulphur quantum dot to the cobalt ions in solution to be measured with the presence or absence of calcium
Ion first separates calcium ion if there are calcium ions in solution to be measured, to avoid calcium ion to sulphur quantum dots characterization
Influence in the process.For example, the mode that the addition carbonate into solution to be measured can be used separates calcium ion.
In addition, its corresponding fluorescence emission spectrum of the calcium chloride solution containing cobalt ions and sulphur quantum dot is further scanned,
Excitation wavelength setting when scanning, the initial value of launch wavelength are 390nm, stop value 440nm, obtained result such as Fig. 7 institute
Show, it is also seen that calcium ion is affected from Fig. 7.
Embodiment 6: the fluorescence invertibity of sulphur quantum dot and cobalt ions detection
Embodiment 6 may include: that circulation executes 5 following steps, it is every has executed it is primary be then poured out it is molten in cuvette
Liquid, and cuvette 5 times wash with distilled water；
Step A6: the sulphur quantum dot of 2mL distilled water and 50 μ L in cuvette, balance is surveyed after five minutes measures it in 360nm
Fluorescence intensity under excitation wavelength surveys primary, measurement 5 times altogether every 5min later.
Step B6: being added 200 μ L cobalt ions solution into the solution after step A6 measurement, balance measured after five minutes its
Fluorescence intensity under 360nm excitation wavelength surveyed primary, measurement 5 times altogether every five minutes later.
The measurement result of embodiment 6 is as shown in figure 8, every the fluorescence intensity of the 5min sulphur quantum dot measured in distilled water
It is roughly the same, it is added after cobalt ions, the fluorescence intensity of sulphur quantum dot is decreased obviously, but every sulphur quantum dot is measured after 5min
Fluorescence intensity tend towards stability, repetitive operation has five circulations altogether, and each loop-around data is almost the same, illustrates that sulphur quantum dot is being examined
When surveying cobalt ions, fluorescence intensity larger floating will not occur as time increases, so cobalt ions is for sulphur quantum dot
Response have invertibity.
It can be seen that sulphur quantum dot after detecting the solution to be measured containing cobalt ions from the testing result of embodiment 6, fluorescence
Strength reduction, and will not increase at any time and restore, therefore, need to be molten to sample in order to restore the fluorescence intensity of sulphur quantum dot
Other substances are added in liquid.
In embodiments of the present invention, by the way that Norfloxacin solution is added into the sample solution containing cobalt ions, can restore
The fluorescence intensity of the sulphur quantum dot of cobalt ions solution was detected, it can be again to Co2+It is detected.Specifically, 0.0319g is taken
Norfloxacin capsule be made into the solution of 0.001mol/L.Norfloxacin solution is added in the system of sulphur quantum dot and cobalt ions
The fluorescence intensity of 20 μ L, discovery sulphur quantum dot increase, and sequentially add 20 μ L Norfloxacin solution, measure its fluorescence emission spectrum
As shown in Figure 9.Wherein, the concentration (mol/L) of the corresponding Norfloxacin in 1 to 20 identified in Fig. 9 is successively are as follows: 0,10-5, 2 ×
10-5, 3 × 10-5, 4 × 10-5, 5 × 10-5, 6 × 10-5, 7 × 10-5, 8 × 10-5, 9 × 10-5, 10-4, 1.1 × 10-4, 1.2 × 10-4, 1.3 × 10-4, 1.4 × 10-4, 1.5 × 10-4, 1.6 × 10-4, 1.7 × 10-4, 1.8 × 10-4, 1.9 × 10-4, 2 × 10-4, i.e.,
The concentration of 1 corresponding Norfloxacin is 0.From fig. 9, it can be seen that with the increase of blood concentration norfloxacin, sulphur quantum dot and cobalt from
The fluorescence intensity of sulphur quantum dot in subsystem gradually increases, and illustrates that Norfloxacin can restore sulphur quantum dot to Co2+Detection it is living
Property.
In addition, further to point of the fluorescence intensity at 410nm in the corresponding fluorescence spectrum of the Norfloxacin of various concentration
Analysis, can obtain blood concentration norfloxacin-fluorescence intensity relational graph as shown in Figure 10.As can be seen from Figure 10 blood concentration norfloxacin with
There are linear relationships between the fluorescence intensity of sulphur quantum dot: F2=359.79632+2.85108 × 10-6C2, wherein F2Characterization adds
Fluorescence intensity of the sample solution under 360nm excitation wavelength after entering the target solution, C2Characterize the Norfloxacin solution
Concentration.From Figure 10 it can also be seen that with blood concentration norfloxacin increase, sulfur content in sulphur quantum dot and cobalt ions system
The fluorescence intensity of son point gradually increases, this also illustrates that Norfloxacin can restore the fluorescence intensity of sulphur quantum dot.
Cobalt ions is first detected using sulphur quantum dot as a result, cobalt ions makes the fluorescent quenching of sulphur quantum dot, to detect
Cobalt ions out.Then the solution relay containing cobalt ions and sulphur quantum dot is utilized to identify that Norfloxacin, Norfloxacin can restore sulphur
The fluorescence intensity of quantum dot, to identify Norfloxacin.This may be to form coordinate bond with Norfloxacin due to cobalt ions,
So that the aggregation inducing effect between cobalt ions and sulphur quantum dot disappears, so that the fluorescence intensity of sulphur quantum dot is extensive
Multiple, it is shown that the reaction mechanism is as follows.This alternatively bright Norfloxacin can be used as sulphur quantum dot formed with cobalt ions it is novel
Thus the switch of sensor can construct a kind of for detecting novel " on-off-on " optical sensing of cobalt ions and Norfloxacin
Device, to make up the defects of conventional method measurement sensitivity is low, time-consuming, accuracy is poor.
According to above scheme, the present invention is at least had the following beneficial effects:
1, sulphur quantum dot in embodiments of the present invention, is added into solution to be measured, sample solution is formed, then by sky
White solution and sample solution carry out fluorescence emission spectrum scanning respectively, do not occur when in the fluorescent emission spectrum of sample solution
When the wave crest occurred in the blank fluorescence emission spectrum of blank solution, that is, it can determine in solution to be measured and contain cobalt ions.In addition, Na+、Fe3+、Cu2+、Mg2+、Zn2+、Pb2+、Cd2+、NH4 +、Ag+、Ni2+And Bi3+Fluorescence emission spectrum there is blank fluorescence hair
The wave crest in spectrum is penetrated, thus illustrates that sulphur quantum dot has feature sensitivities to cobalt ions, the detection of cobalt ions can be used for.
2, in embodiments of the present invention, directly the cobalt ions in solution to be measured can be detected using sulphur quantum dot, and
It is not necessary that other cations in solution to be measured are sheltered or separated, so as to shorten the detection duration of cobalt ions.
3, in embodiments of the present invention, by the way that sulphur quantum dot to be dissolved in the solution of different concentration of cobalt ions, and respectively
The fluorescence intensity of solution is detected, to detect the fluorescence intensity change of sulphur quantum dot under the influence of different concentration of cobalt ions.Detection
The result shows that concentration of cobalt ions and the fluorescence intensity of sulphur quantum dot have good linear relationship, using the linear pass measured
System directly calculates the concentration of cobalt ions in solution to be measured, simplifies the detection process of concentration of cobalt ions.
4, in embodiments of the present invention, sulphur quantum dot has good invertibity to the sensing of cobalt ions, using promise fluorine
Sha Xing restores sulphur quantum dot to the detection activity of cobalt ions, so that sulphur quantum dot can repeated detection solution to be measured.
5, the novel sensor in embodiments of the present invention, formed using Norfloxacin as sulphur quantum dot with cobalt ions is opened
It closes, thus can construct a kind of for detecting novel " on-off-on " optical sensor of cobalt ions and Norfloxacin, compensate for biography
The defects of system method measurement sensitivity is low, time-consuming, accuracy is poor.
It should be noted that, in this document, such as first and second etc relational terms are used merely to an entity
Or operation is distinguished with another entity or operation, is existed without necessarily requiring or implying between these entities or operation
Any actual relationship or order.Moreover, the terms "include", "comprise" or its any other variant be intended to it is non-
It is exclusive to include, so that the process, method, article or equipment for including a series of elements not only includes those elements,
It but also including other elements that are not explicitly listed, or further include solid by this process, method, article or equipment
Some elements.In the absence of more restrictions, the element limited by sentence " including one ", is not arranged
Except there is also other identical factors in the process, method, article or apparatus that includes the element.
Finally, it should be noted that the foregoing is merely presently preferred embodiments of the present invention, it is merely to illustrate skill of the invention
Art scheme, is not intended to limit the scope of the present invention.Any modification for being made all within the spirits and principles of the present invention,
Equivalent replacement, improvement etc., are included within the scope of protection of the present invention.
Claims (8)
1. a kind of method using sulphur quantum dots characterization cobalt ions characterized by comprising
The sulphur quantum dot of the first mass parts is dissolved in distilled water respectively, forms blank solution；
The sulphur quantum dot of second mass parts is dissolved in solution to be measured, sample solution is formed；
Further include:
The blank solution is scanned under 360nm excitation wavelength by sepectrophotofluorometer, within the scope of 380nm~450nm
Blank fluorescence emission spectrum；
The sample solution is scanned under 360nm excitation wavelength by sepectrophotofluorometer, within the scope of 380nm~450nm
Fluorescent emission spectrum；
When the fluorescent emission spectrum wave crest does not occur within the scope of 395nm~415nm, determine in the solution to be measured
Contain cobalt ions；Wherein, the wave crest appears within the scope of 395nm~415nm of the blank fluorescence emission spectrum.
2. the method according to claim 1, wherein
It is described the sulphur quantum dot of second mass parts is dissolved in solution to be measured before, further comprise: described in adjusting
The pH of solution to be measured is 7~8.
3. the method according to claim 1, wherein
Containing after cobalt ions in the determination solution to be measured, further comprise:
The fluorescence intensity of the sample solution and blank solution under 360nm excitation wavelength is detected respectively；
According to the following formula, the concentration of cobalt ions in the solution to be measured is calculated；
F0/F1=5.73194+9325C1
Wherein, F1Characterize fluorescence intensity of the sample solution at 360nm, F0It is glimmering at 360nm to characterize the blank solution
Luminous intensity, C1Characterize the concentration of cobalt ions in the solution to be measured.
4. the method according to claim 1, wherein
The sulphur quantum dot of second mass parts is dissolved in solution to be measured described, is formed before sample solution, further
Include:
It detects with the presence or absence of calcium ion in the solution to be measured, if so, being separated to the calcium ion in the solution to be measured.
5. the method according to claim 1, wherein
When the volume of the distilled water is equal with the volume of the solution to be measured, first mass parts and second mass
Part is equal.
6. a kind of method using sulphur quantum dot relay identification Norfloxacin characterized by comprising
When determining fluorescent emission spectrum within the scope of 395nm~415nm using any method of claim 1 to 5
When not occurring wave crest, further includes:
Target solution is added into sample solution；
Through the sample solution after the sepectrophotofluorometer scanning addition target solution under 360nm excitation wavelength,
Target fluorescent emission spectrum within the scope of 380nm~450nm；
When the fluorescence intensity in the target fluorescent emission spectrum is greater than in the fluorescent emission spectrum under corresponding wavelength
It when fluorescence intensity, determines and contains Norfloxacin in the target solution, and restore the sulphur quantum dot in the sample solution to cobalt
The detection activity of ion.
7. according to the method described in claim 6, it is characterized in that,
Containing after Norfloxacin in the determination target solution, further comprise:
Fluorescence intensity of the sample solution under 360nm excitation wavelength after the detection addition target solution；
According to following calculation formula, the concentration of the Norfloxacin solution is calculated；
F2=359.79632+2.85108 × 10-6C2
Wherein, F2Fluorescence intensity of the sample solution under 360nm excitation wavelength after the characterization addition target solution, C2Characterization
The concentration of the Norfloxacin solution.
8. according to the method described in claim 6, it is characterized in that,
After the determining fluorescent emission spectrum wave crest does not occur within the scope of 395nm~415nm, described to described
It is added before target solution in sample solution, further comprises:
According to preset period of time, fluorescence intensity of the sample solution under 360nm excitation wavelength is detected；
Determine the strength difference between the corresponding fluorescence intensity of each time cycle；
When the strength difference is less than preset threshold, execution is described to be added target solution into the sample solution.
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