CN106769613B - A kind of preparation of the potassium ion sensor based on QCM - Google Patents
A kind of preparation of the potassium ion sensor based on QCM Download PDFInfo
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- CN106769613B CN106769613B CN201710025955.6A CN201710025955A CN106769613B CN 106769613 B CN106769613 B CN 106769613B CN 201710025955 A CN201710025955 A CN 201710025955A CN 106769613 B CN106769613 B CN 106769613B
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Abstract
The present invention relates to the potassium ion sensors and its preparation method and application based on quartz crystal microbalance.The quartz crystal of quartz crystal microbalance sensor of the invention is modified with crown ether quasi polymer, is enable to respond quickly, and detects potassium concentration.
Description
Technical field
The invention belongs to biomedicine fields, and in particular to one kind is passed based on the potassium ion of QCM (quartz crystal microbalance)
Sensor and its preparation and detection method.
Background technique
Potassium ion is the dominant cation of intracellular fluid, and internal 98% potassium is present in into the cell.Potassium ion, which has, to be maintained
The activity of the function of cell metabolism, intracellular some enzymes must form Shi Youyi with the presence of the potassium ion of high concentration, glycogen
Quantitative potassium ion enters into the cell, and protein synthesis and decomposition are shifted with a certain amount of potassium ion；Potassium ion, which has, to be maintained
The function of intraor extracellular osmotic pressure and acid-base balance, when low potassium, are easy to happen metabolic alkalosis；Potassium ion, which has, keeps mind
Through muscle irritability performance, blood potassium is excessively high, then neuromuscular is overexcited, hypokalemia, then neuromuscular paralysis；Potassium ion tool
There is the coordination for maintaining normal myocardium contractile motion, blood potassium is excessively high, can inhibit cardiac muscle, and such as hypokalemia then generates arrhythmia.Institute
It must be maintained in a metastable concentration range (3.5~5.5mM) with human body potassium ion.
In conclusion the intracorporal potassium of people is the dominant cation for maintaining cellular physiological events, it is to maintain the normal infiltration of body
Pressure and acid-base balance thoroughly participate in sugar and protein metabolism, guarantee that nervimuscular normal function institute is required, content is that human body is raw
Manage movable important indicator.The some kidneys of diagnosis, heart etc. has clinically can be used in the contents level of potassium ion in urine, serum
The disease of aspect.Therefore the concentration of potassium ion has very important influence to human health, realizes quick, portable detection potassium
The concentration of ion has very important significance.At present the method for accurate detection potassium ion substantially have it is several under it is several: 1. biochemical points
Analyzer is the instrument that certain specified chemical ingredient in body fluid is measured using photoelectric colorimetry principle；2. blomelicalbloodgasandelectrolrteanalyzers are to adopt
It is realized with ion-selective electrode mensuration and accurately to be detected；3. Atomic Absorption Spectrometer is based on outside gaseous ground state atom
Layer electronics is quantitatively tested constituent content to the absorption intensity of the corresponding atomic resonance radiation of ultraviolet light and visible-range
Based on analysis method.Though the method for detecting potassium ion is more, equipment instrument is larger, analysis time length etc., it is difficult to meet
Real-time test, the especially clinical detection for needing to carry out Cavity in Critical Patients fast potassium.
Summary of the invention
On the one hand the purpose of the present invention is to provide a kind of potassium ion sensor based on quartz crystal microbalance, the biography
The quartz crystal of sensor is modified with crown ether quasi polymer.
Preferably, the crown ether quasi polymer comprises the following steps:
By acrylamide 15mg, polyethylene glycol dimethacrylate 6mg, 2,2- dimethoxy-phenylf ethyl ketone 1mg, N-
N'- methylene-bisacrylamide 2mg, 2- allyloxy methyl 18- crown- 6- ether 5mg is dissolved in 60uL dimethyl sulfoxide and crown ether is made
Quasi polymer.
On the one hand the purpose of the present invention is to provide a kind of preparation of potassium ion sensor based on quartz crystal microbalance
Method, the preparation method comprises the following steps:
(1) quartz crystal is respectively in dense H2SO4And H2O2(V:V=7:3), acetone, ethyl alcohol, 10 points of ultrasound in ultrapure water
Clock is dried with nitrogen；
(2) the processed quartz crystal of step (1) is immersed into (γ containing 150uL-aminopropyl three in 30ml analysis straight alcohol
Ethoxysilane) it impregnates for 24 hours, it is dried with nitrogen；
(3) step (2) processed quartz crystal is placed in 25mlN, (it is suitable contains 1g in N ˊ-dimethyl formamide solution
Anhydride maleique) it impregnates for 24 hours, it is dried with nitrogen；
(4) by acrylamide 15mg, polyethylene glycol dimethacrylate 6mg, 2,2- dimethoxy-phenylf ethyl ketone 1mg,
N-N'- methylene-bisacrylamide 2mg, 2- allyloxy methyl 18- crown- 6- ether 5mg, which is dissolved in 60uL dimethyl sulfoxide, to be made
Crown ether quasi polymer；
(5) take 20-30uL, preferably 25uL crown ether-like polymer drops in the processed quartz crystal oscillator on piece of step (3),
The polymer-modified quartz crystal microbalance of crown ether-like can be obtained in 4000r/min spin coating 1min, ultraviolet 365nm illumination 30min
Potassium ion sensor.
The purpose of the present invention on the one hand be to provide the application of the potassium ion sensor based on quartz crystal microbalance, wherein
The potassium ion sensor of the quartz crystal microbalance is used to detect the potassium ion of low concentration.
Preferably, the lowest detection of the potassium concentration is limited to 0.5mmol/L.
Preferably, the method for the detection are as follows:
(1) it takes the polymer-modified good crystal-vibration-chip of crown ether-like to detect its frequency in quartz crystal microbalance, is denoted as F0.
(2) potassium ion solution of various concentration is added, concentration range 0.5-7mmol/L detects its frequency, is denoted as F1.
(3) step (1) and step (2) are pressed, the frequency variation of the corresponding crystal-vibration-chip of potassium ion solution of various concentration is obtained
Y, and mapped with the potassium ion of various concentration with corresponding frequency shifting, draw standard curve, regression equation Y=-
37.47LgC+59.74, in which: Y is frequency variation, and unit Hz, LgC are potassium concentration logarithm.Frequency is in log concentration
Linear relationship, degree of fitting 0.9624, obtained standard curve are as shown in Figure 3.
(4) solution to be measured is tested into its Y by step described in step (3)；Reference standards curve obtains in solution to be measured
Potassium concentration.
It should be appreciated that aforementioned description substantially and subsequent detailed description are exemplary illustration and explanation, it should not
As the limitation to the claimed content of the present invention.
Detailed description of the invention
With reference to the attached drawing of accompanying, the more purposes of the present invention, function and advantage are by the as follows of embodiment through the invention
Description is illustrated, in which:
Fig. 1 is the pictorial diagram of QCM potassium ion sensor of the invention；
Fig. 2 is the synthetic route chart of QCM potassium ion sensor of the invention；
Fig. 3 is the frequency variation curve figure of the corresponding crystal-vibration-chip of potassium ion solution of various concentration；
Fig. 4 is the potassium ion detection range and the schematic diagram of response time of QCM potassium ion sensor of the invention；
Fig. 5 is the selective experimental result schematic diagram of QCM potassium ion sensor of the invention to different ions.
Specific embodiment
By reference to exemplary embodiment, the purpose of the present invention and function and the side for realizing these purposes and function
Method will be illustrated.However, the present invention is not limited to exemplary embodiment as disclosed below；Can by different form come
It is realized.The essence of specification is only to aid in those skilled in the relevant arts' Integrated Understanding detail of the invention.
Hereinafter, the embodiment of the present invention will be described with reference to the drawings.In the accompanying drawings, identical appended drawing reference represents identical
Or similar component or same or like step.
The present invention proposes a kind of potassium ion detection method based on QCM, using crown ether derivative as the identification of potassium ion
Unit realizes that crown ether polymer in the polymerization of quartz crystal oscillator on piece, realizes the on-line checking of potassium ion using surface initiation polymerization.
The pictorial diagram of potassium ion sensor based on QCM is as shown in Figure 1.
The above-mentioned potassium ion sensor based on QCM is prepared by following methods, and specific step is as follows, and synthetic route is as schemed
Shown in 2:
(1) quartz crystal is respectively in dense H2SO4And H2O2(V:V=7:3), acetone, ethyl alcohol, 10 points of ultrasound in ultrapure water
Clock is dried with nitrogen, in Fig. 2 shown in (a)；
(2) the processed quartz crystal of step (1) is immersed into (γ containing 150uL-aminopropyl three in 30ml analysis straight alcohol
Ethoxysilane) it impregnates for 24 hours, it is dried with nitrogen, in Fig. 2 shown in (b)；
(3) step (2) processed quartz crystal is placed in 25mlN, (it is suitable contains 1g in N ˊ-dimethyl formamide solution
Anhydride maleique) it impregnates for 24 hours, it is dried with nitrogen, in Fig. 2 shown in (c)；
(4) by acrylamide 15mg, polyethylene glycol dimethacrylate 6mg, 2,2- dimethoxy-phenylf ethyl ketone 1mg,
N-N'- methylene-bisacrylamide 2mg, 2- allyloxy methyl 18- crown- 6- ether 5mg, which is dissolved in 60uL dimethyl sulfoxide, to be made
Crown ether quasi polymer；
(5) take 20-30uL, preferably 25uL crown ether-like polymer drops in the processed quartz crystal oscillator on piece of step (3),
The polymer-modified QCM potassium ion sensing of crown ether-like can be obtained in 4000r/min spin coating 1min, ultraviolet 365nm illumination 30min
Device, in Fig. 2 shown in (d).
Potassium ion sensor based on QCM of the invention can be used for detecting the concentration of potassium ion, the detection method are as follows:
(1) crystal-vibration-chip for taking above-mentioned modification good detects its frequency in QCM, is denoted as F0.
(2) potassium ion solution of various concentration is added, concentration range 0.5-7mmol/L detects its frequency, is denoted as F1.
(3) step (1) and step (2) are pressed, the frequency variation of the corresponding crystal-vibration-chip of potassium ion solution of various concentration is obtained
Y, and mapped with the potassium ion of various concentration with corresponding frequency shifting, draw standard curve, regression equation Y=-
37.47LgC+59.74, in which: Y is frequency variation, and unit Hz, LgC are potassium concentration logarithm.Frequency is in log concentration
Linear relationship, degree of fitting 0.9624, obtained standard curve are as shown in Figure 3.
(4) solution to be measured is tested into its Y by step described in step (3)；Reference standards curve obtains in solution to be measured
Potassium concentration.
Fig. 4 is the potassium ion detection range and the schematic diagram of response time of QCM potassium ion sensor of the invention.From Fig. 4
In as can be seen that the potassium ion sensor of the invention based on QCM potassium ion range that can be detected between 0.5-7mM, most
Low detection limit can reach 0.5mmol/L, and the response time is 30s, can be quickly detected the concentration of potassium ion.
Fig. 5 is the detection Choice tests of the invention detected based on the sensor of QCM to lead ion, prepares concentration respectively
For the sodium of 4mmol/L, calcium, magnesium, ammonium root solion, using test method of the invention detect its frequency change, and with it is dense
Degree is that the lead ion solution of 4mmol/L is compared.The result shows that concentration is the sodium of 4mmol/L, the ion pair of calcium, magnesium, ammonium root
The potassium ion solution that the frequency variation of measurement system is all significantly less than 4mmol/L changes the frequency of measurement system, to show
Sensor of the invention is preferable to potassium ion selective, has specificity.Work as Na+、Ca2+、Mg2+Deng in the presence of, still can quickly,
Potassium ion is recognized accurately.
A kind of potassium ion detection method based on QCM proposed by the present invention, using crown ether derivative as the knowledge of potassium ion
Other unit, has the advantage that
1. detecting instrument category portable instrument, achievable instant detection；
2. meeting the potassium ion detection of Human Physiology range；
3. quick response；
4. other ions of pair human body, such as Na+、Ca2+、Mg2+With preferable screen effect.
(remarks: the solution of unmarked concentration is the commercially available pure solution of analysis in text, and reagent is that commercially available analysis is pure.)
In conjunction with the explanation and practice of the invention disclosed here, the other embodiment of the present invention is for those skilled in the art
It all will be readily apparent and understand.Illustrate and embodiment is regarded only as being exemplary, true scope of the invention and purport are equal
It is defined in the claims.
Claims (5)
1. a kind of potassium ion sensor based on quartz crystal microbalance, the quartz crystal of the sensor are modified with crown ether-like
Polymer；
Wherein the crown ether-like polymer comprises the following steps:
Acrylamide 15mg, polyethylene glycol dimethacrylate 6mg, 2,2- dimethoxy-phenylf ethyl ketone 1mg, N-N'- is sub-
Bisacrylamide 2mg, 2- allyloxy methyl 18- crown- 6- ether 5mg is dissolved in 60uL dimethyl sulfoxide and crown ether Type of Collective is made
Object.
2. a kind of preparation method of the potassium ion sensor described in claim 1 based on quartz crystal microbalance, the preparation
Method the following steps are included:
(1) quartz crystal is in dense H2SO4And H2O2, acetone, ethyl alcohol, ultrasound 10 minutes in ultrapure water, be dried with nitrogen, it is described dense
H2SO4And H2O2V:V=7:3；
(2) the processed quartz crystal of step (1) is immersed in 30ml analysis straight alcohol and is impregnated for 24 hours, the analysis straight alcohol
Gamma-aminopropyl-triethoxy-silane containing 150uL is dried with nitrogen；
(3) step (2) processed quartz crystal is placed in 25mlN, is impregnated for 24 hours in N ˊ-dimethyl formamide solution, it is described
N, N ˊ-dimethyl formamide solution maleic anhydride containing 1g, are dried with nitrogen；
(4) by acrylamide 15mg, polyethylene glycol dimethacrylate 6mg, 2,2- dimethoxy-phenylf ethyl ketone 1mg, N-
N'- methylene-bisacrylamide 2mg, 2- allyloxy methyl 18- crown- 6- ether 5mg, which is dissolved in 60uL dimethyl sulfoxide, is made hat
Ether polymer；
(5) take 20-30uL crown ether-like polymer drops in the processed quartz crystal oscillator on piece of step (3), 4000r/min spin coating
The polymer-modified quartz crystal microbalance potassium ion sensor of crown ether-like can be obtained in 1min, ultraviolet 365nm illumination 30min.
3. a kind of application of the potassium ion sensor described in claim 1 based on quartz crystal microbalance, wherein the quartz
The potassium ion sensor of crystal microbalance is used to detect the potassium ion of low concentration.
4. application according to claim 3, wherein the lowest detection of the potassium concentration is limited to 0.5mmol/L.
5. application according to claim 3 or 4, wherein the method for the detection are as follows:
(1) it takes the polymer-modified good crystal-vibration-chip of crown ether-like to detect its frequency in quartz crystal microbalance, is denoted as F0；
(2) potassium ion solution of various concentration is added, concentration range 0.5-7mmol/L detects its frequency, is denoted as F1；
(3) step (1) and step (2) are pressed, the frequency variation Y of the corresponding crystal-vibration-chip of potassium ion solution of various concentration is obtained, and
Changed with the potassium ion of various concentration with corresponding frequency and mapped, draws standard curve, regression equation Y=-37.47LgC+
59.74, in which: Y is frequency variation, and unit Hz, LgC are potassium concentration logarithm；Frequency is in a linear relationship with log concentration,
Degree of fitting is 0.9624, obtains the frequency variation canonical plotting of the corresponding crystal-vibration-chip of potassium ion solution of various concentration；
(4) solution to be measured is tested into its Y by step described in step (3)；Reference standards curve obtain the potassium in solution to be measured from
Sub- concentration.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85205673U (en) * | 1985-12-11 | 1988-02-10 | 南京大学 | Potassium ion sensor of semiconductor |
| JPH03282348A (en) * | 1990-03-30 | 1991-12-12 | Sanyo Electric Co Ltd | Detecting element |
| WO2002023176A1 (en) * | 2000-09-13 | 2002-03-21 | British Nuclear Fuels Plc | Improvements in and relating to sensors |
| CN101294927A (en) * | 2007-04-27 | 2008-10-29 | 株式会社日立高新技术 | Ion concentration measuring device and ion concentration measuring element |
| CN101871912A (en) * | 2010-06-07 | 2010-10-27 | 浙江大学 | Full-solid potassium ion sensor and preparation method thereof |
-
2017
- 2017-01-13 CN CN201710025955.6A patent/CN106769613B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85205673U (en) * | 1985-12-11 | 1988-02-10 | 南京大学 | Potassium ion sensor of semiconductor |
| JPH03282348A (en) * | 1990-03-30 | 1991-12-12 | Sanyo Electric Co Ltd | Detecting element |
| WO2002023176A1 (en) * | 2000-09-13 | 2002-03-21 | British Nuclear Fuels Plc | Improvements in and relating to sensors |
| CN101294927A (en) * | 2007-04-27 | 2008-10-29 | 株式会社日立高新技术 | Ion concentration measuring device and ion concentration measuring element |
| CN101871912A (en) * | 2010-06-07 | 2010-10-27 | 浙江大学 | Full-solid potassium ion sensor and preparation method thereof |
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