CN107576636A - With tetraphenylboron sodium part regulation and control stannic oxide/graphene nano band catalytically active surface plasmon absorption spectroscopic assay K+Method - Google Patents
With tetraphenylboron sodium part regulation and control stannic oxide/graphene nano band catalytically active surface plasmon absorption spectroscopic assay K+Method Download PDFInfo
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Abstract
The invention discloses one kind tetraphenylboron sodium part regulation and control stannic oxide/graphene nano band catalytically active surface plasmon absorption spectroscopic assay K+Method, it is characterized in that, comprise the following steps：（1）Prepare the K of concentration known+Standard liquid system；（2）Prepare placebo solution system；（3）Calculate Δ A=A A0；（4）With Δ A to K+Concentration relationship work curve；（5）Calculate Δ ASample=ASample‑ A0；（6）According to step（4）Working curve, calculate sample solution K+Content.This assay method is using part regulation and control nanometer enzymatic activity, and method is easy, quick, high sensitivity.
Description
Technical field
The present invention relates to analytical chemistry field, is specifically that one kind is urged with tetraphenylboron sodium part regulation and control stannic oxide/graphene nano band
Change active surface plasmon absorption spectrum (Surface Plasmon Resonance, abbreviation SPR) measure K+Side
Method.
Background technology
Potassium ion (K+) it is a kind of important physiologic elements, with Na+Collective effect, maintaining cell metabolism, regulation body
Liquid osmotic pressure, maintain acid-base balance and keep cellular stress function etc. to play extremely important effect, meanwhile, potassium ion
Different effects, including neurotransmission are played during biological growth, enzyme activation, Apoptosis, is adjusted in blood pressure and cell
Other ions concentration, into the cell between extracellular liquid K+The disorder of ion concentration is always relevant with a series of diseases,
Including alcoholism, apocleisis, bulimia nerovsa, AIDS and kidney trouble, therefore, K+The detection of ion has become one very
The problem of important.The conventional method of measure potassium has：Flame spectrometry, fluorescence spectrophotometric method, atomic absorption spectrography (AAS), current potential
Titration etc. and surface plasmon absorption spectroscopic methodology, but the most complex operation of these methods, ion interference is big, influence because
Element is more, and sensitivity is not high enough, and accuracy is not good enough, therefore, it is desirable to develop a kind of simple, sensitive, economic and effective inspection
Survey K+The method of the wide range of linearity of ion.
With the high speed development of nano science, China scientist has found that inorganic nano material has inherent similar horseradish in itself
The catalytic activity of peroxidase (HRP), its catalytic efficiency and mechanism of action are similar to native enzyme.Horseradish peroxidase is one
Kind very important metalloproteinases, is widely used in the multiple fields such as chemical industry, food, medical science, environment, the appearance of nano enzyme,
Cause the great attention of the multiple fields scientist such as physics, material, chemistry, biology and medical science, its analogue enztme new as one kind,
Have become the study hotspot of multi-crossed disciplines, and gradually formed new research field, based on Fe3O4The peroxide of nano particle
Compound enzymatic property, the quantitative analysis of hydrogen peroxide can be realized by the change of some substrate colors.Electrum nano flower particle,
Because the nano flower particle of synthesis has higher Mimetic Peroxidase activity, and with good surface enhanced scattering base
Bottom, the detection and analysis of melamine are thus be accordingly used in, utilize heavy metal particles Hg2+Addition and peroxidase activity enhancing
Quantitative relationship be present, so as to realize to Hg2+Analysis detection.Generally, large biological molecule often covers the surface of nano material,
The atom of nano-material surface and the contact area by catalysis substrate can be greatly increased, so as to reduce the activity of nano enzyme, by
In such mechanism, using fibrinogen modification bismuth gold nano grain and be used as H2O2Analogies and Amplex Red are anti-
Should, for determining thrombin activity and drug screening, realize the quantitative detection of fibrin ferment.Possesses the nanometer of oxide enzymatic property
Cerium material, nano cerium replacement HRP is used into ELISA method detection cancer cell.Graphene nanobelt is received by the more wall carbon of oxidative cleavage
What mitron was prepared, show the catalysis characteristics of more preferable nano enzyme.Surface plasmon absorption (SPR) is according to incident
Light is irradiated to caused by the dielectric surface of different refractivity metal free electron from critical angle and resonated, and obtains mutual between molecule
Action specificity signal to carry out qualitative and quantitative analysis to molecular components.But application tetraphenylboron sodium regulation and control stannic oxide/graphene nano
Band catalytic activity measure K+The method of surface plasmon absorption spectrum have not been reported.
The content of the invention
The purpose of the present invention is for measure K+The deficiencies in the prior art, and a kind of tetraphenylboron sodium part regulation and control oxygen is provided
Graphite alkene nanobelt catalytically active surface plasmon absorption spectroscopic assay K+Method.This method is anti-using part
A nanometer enzymatic activity should be regulated and controled, method is easy, quick, high sensitivity.
Realizing the technical scheme of the object of the invention is：
One kind tetraphenylboron sodium part regulation and control stannic oxide/graphene nano band catalytically active surface plasmon absorption light
Spectrum measure K+Method, comprise the following steps：
(1) K of concentration known is prepared+Standard liquid system：In scale test tube, the μ of 10 μ L-400 μ L 10 are sequentially added
Mol/L K+Standard liquid, 100 μ L-180 μ L 47.5ng/mL stannic oxide/graphene nanos bands, 300 10 μm of ol/L of μ L-500 μ L
Sodium tetraphenylborate solution, 30 μ L-100 μ L 0.3mol/L glucose, 100 μ L-200 μ L 1mmol/L AgNO3With 10 μ L-50
μ L 0.5mol/L NaOH solutions, in 60 DEG C of water-baths 5 minutes, shake up, then frozen water is cooled to room temperature, adds 80 μ L-150
μ L 1mol/L NaCl, 2.0mL is settled to redistilled water；
(2) placebo solution system is prepared：K is not added with the method for step (1)+Standard liquid prepares placebo solution
System；
(3) K by step (1), (2) preparation is taken respectively+Standard liquid system and placebo solution system are poured into colorimetric
In ware, on spectrophotometer, instrument parameter is set, scans the surface plasmon absorption spectrum of acquisition system, measure
Absorbance at 410nm is A, while the absorbance for determining placebo solution system is A0, calculate Δ A=A-A0；
(4) with Δ A to K+Concentration relationship work curve；
(5) method according to step (1) prepares sample solution, wherein the K added+Standard liquid replaces with sample solution,
And the absorbance for pressing the method determination sample solution of step (3) is ASample, calculate Δ ASample=ASample-A0；
(6) working curve according to step (4), calculates sample solution K+Content.
The preparation method of stannic oxide/graphene nano band is described in step (1)：
1) 50mg multi-walled carbon nanotubes are taken, i.e. MWCNT powder is added to containing the dense H of 10mL2SO450mL round-bottomed flasks in
Reaction 1 hour, then add 250mg KMnO4；
2) after solution prepared by step 1) is fully shaken up under 60 DEG C of water bath conditions heating response 2 hours, then by product
Pour into containing 5mL 30%H2O2200mL frozen water in cool down；
3) reacted solution will be cooled down, ultrasonic disperse centrifuges 10 minutes under 7000 rotating speeds after 10 minutes, takes supernatant
Liquid, the manganese dioxide of reaction generation is removed, finally obtain stannic oxide/graphene nano band solution.
Stannic oxide/graphene nano band solution is then diluted in use, be first neutralized to neutrality with 50mmol/L NaOH
Required concentration.
Under the conditions of the technical program, stannic oxide/graphene nano band is to glucose-AgNO3Generating Nano silver grain, this is anti-
There should be stronger catalytic action；When tetraphenylboron sodium is wrapped in stannic oxide/graphene nano band nano enzyme surface, it is suppressed that grape
Sugar-AgNO3This reaction of generation Nano silver grain；When system adds K+When, K+Generation potassium tetraphenylborate is reacted with tetraphenylboron sodium, i.e.,
(C6H5)4BK, and depart from from stannic oxide/graphene nano band nano enzyme surface, stannic oxide/graphene nano band catalytic activity is recovered.System
In with K+The increase of concentration, stannic oxide/graphene nano band catalytic activity strengthen, and the Nano silver grain of generation increases；Absorbance
Increase.K+Concentration and system absorbance enhancement value are in certain linear relationship, establish measure K accordingly+Tetraphenylboron sodium regulation and control oxidation
Graphene nanobelt active surface plasmon absorption spectrographic technique.
The advantages of this method is：Compared with the existing methods, this assay method is lived using part regulation and control nanometer enzymatic
Property, method is easy, quick, high sensitivity.
Brief description of the drawings
Fig. 1 is the surface plasmon absorption spectrogram in embodiment.
In figure, a.3.56ng/mL+2 μm of ol/L (C of stannic oxide/graphene nano band6H5)4The μ of BNa+7.5mmol/L glucose+75
mol/L AgNO3+6.25mmol/L NaOH+50mmol/L NaCl b.a+0.05μmol/L K+ c.a+0.75μmol/L K+
d.a+1.25μmol/L K+ e.a+1.5μmol/L K+ f.a+2.0μmol/L K+。
Embodiment
Present invention is further elaborated with reference to embodiment and accompanying drawing, but is not limitation of the invention.
Embodiment：
One kind tetraphenylboron sodium part regulation and control stannic oxide/graphene nano band catalytically active surface plasmon absorption light
Spectrum measure K+Method, comprise the following steps：
(1) K of concentration known is prepared+Standard liquid system：In 5 scale test tubes, be separately added into 10 μ L, 150 μ L,
250 μ L, 300 μ L, 400 10 μm of ol/L of μ L K+150 μ L47.5ng/ are sequentially added in standard liquid and then every scale test tube
ML stannic oxide/graphene nanos band, 400 10 μm of ol/L of μ L sodium tetraphenylborate solution, 50 μ L 0.3mol/L glucose, 150 μ L
1mmol/L AgNO3With 25 μ L 0.5mol/L NaOH solutions, in 60 DEG C of water-baths 5 minutes, shake up, add 100 μ L
1mol/L NaCl, then frozen water be cooled to room temperature, be settled to 2.0mL with redistilled water；
(2) placebo solution system is prepared：K is not added with the method for step (1)+Standard liquid prepares placebo solution
System；
(3) K by step (1), (2) preparation is taken respectively+Standard liquid system and placebo solution system are poured into quartz
In cuvette, on UV-1901 type spectrophotometric spectra meters, set instrument parameter slit as 2nm, scan surface etc. of acquisition system from
Daughter resonance absorbance spectrum such as Fig. 1, the absorbance determined at 410nm is A, while determines the extinction of placebo solution system
Angle value is A0, calculate Δ A=A-A0；
(4) with Δ A to K+Concentration relationship work curve；Acquisition equation of linear regression is Δ A410nm=0.154C+
0.009, wherein K+The unit of concentration C is μm ol/L, and the measure range of linearity is 0.05-2 μm of ol/L, and detection is limited to 0.021 μm of ol/
L；
(5) sample determines：Drinking Water is taken, is measured in right amount, the method according to step (1) prepares sample, wherein
The K of addition+Standard liquid replaces with sample, is operated by step (2)-(4), calculates the Δ A of sampleSample=ASample-A0；
(6) working curve according to step (4), calculates sample K+Content be 0.062 μm of ol/L.
The preparation method of stannic oxide/graphene nano band is described in this example step (1)：
1) 50mg multi-walled carbon nanotubes are taken, i.e. MWCNT powder is added to containing the dense H of 10mL2SO450mL round-bottomed flasks in
Reaction 1 hour, then add 250mg KMnO4；
2) after solution prepared by step 1) is fully shaken up under 60 DEG C of water bath conditions heating response 2 hours, then by product
Pour into containing 5mL 30%H2O2200mL frozen water in cool down；
3) reacted solution will be cooled down, ultrasonic disperse centrifuges 10 minutes under 7000 rotating speeds after 10 minutes, takes supernatant
Liquid, the manganese dioxide of reaction generation is removed, finally obtain stannic oxide/graphene nano band solution.
Stannic oxide/graphene nano band solution is then diluted in use, be first neutralized to neutrality with 50mmol/L NaOH
Required concentration.
The checking of the technical program detection method：
Three parts of water sample in above-described embodiment step (5) is taken, is separately added into K of the concentration for 0.05 μm of ol/L+Standard liquid,
Recovery testu is carried out, it is respectively 98.3%, 96.7%, 99.9% to try to achieve the rate of recovery, relative standard deviation 3.6%.
Illustrate the technical scheme method accurately and reliably.
Claims (1)
1. one kind tetraphenylboron sodium part regulation and control stannic oxide/graphene nano band catalytically active surface plasmon absorption spectrum
Determine K+Method, it is characterized in that, comprise the following steps：
(1) K of concentration known is prepared+Standard liquid system：In scale test tube, sequentially add 10 10 μm of ol/L's of μ L-400 μ L
K+Standard liquid, 100 μ L-180 μ L 47.5ng/mL stannic oxide/graphene nanos bands, 300 10 μm of ol/L of μ L-500 μ L tetraphenylboron
Sodium solution, 30 μ L-100 μ L 0.3mol/L glucose, 100 μ L-200 μ L 1mmol/L AgNO3With 10 μ L-50 μ L
0.5mol/L NaOH solutions, in 60 DEG C of water-baths 5 minutes, shake up, then frozen water is cooled to room temperature, adds 80 μ L-150 μ L
1mol/L NaCl, 2.0mL is settled to redistilled water；
(2) placebo solution system is prepared：K is not added with the method for step (1)+Standard liquid prepares placebo solution system；
(3) K by step (1), (2) preparation is taken respectively+Standard liquid system and placebo solution system are poured into cuvette,
On spectrophotometer, instrument parameter is set, scans the surface plasmon absorption spectrum of acquisition system, determines 410nm
The absorbance at place is A, while the absorbance for determining placebo solution system is A0, calculate Δ A=A-A0；
(4) with Δ A to K+Concentration relationship work curve；
(5) method according to step (1) prepares sample solution, wherein the K added+Standard liquid replaces with sample solution, and by step
Suddenly the absorbance of the method determination sample solution of (3) is ASample, calculate Δ ASample=ASample-A0；
(6) working curve according to step (4), calculates sample solution K+Content.
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| CN107389658A (en) * | 2017-08-16 | 2017-11-24 | 广西师范大学 | One kind tetraphenylboron sodium part regulation and control stannic oxide/graphene nano band catalytically active surface enhancing Raman spectroscopy K+Method |
| CN107389658B (en) * | 2017-08-16 | 2019-08-23 | 广西师范大学 | It is a kind of to enhance Raman spectroscopy K with tetraphenylboron sodium ligand regulation stannic oxide/graphene nano band catalytically active surface+Method |
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