CN104914147B - One kind is based on magnetic Nano NiFe2O4Electrochemical sensor preparation method and application - Google Patents
One kind is based on magnetic Nano NiFe2O4Electrochemical sensor preparation method and application Download PDFInfo
- Publication number
- CN104914147B CN104914147B CN201510270421.0A CN201510270421A CN104914147B CN 104914147 B CN104914147 B CN 104914147B CN 201510270421 A CN201510270421 A CN 201510270421A CN 104914147 B CN104914147 B CN 104914147B
- Authority
- CN
- China
- Prior art keywords
- electrode
- nife
- rutin
- quercetin
- magnetic nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Investigating Or Analyzing Materials By The Use Of Magnetic Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The present invention relates to electrochemical analysis techniques fields, especially a kind of to be based on magnetic Nano NiFe2O4Electrochemical sensor preparation method and application, by glass-carbon electrode and NiFe2O4Dispersion liquid forms, wherein, electrode structure is to coat layer of Ni Fe in glassy carbon electrode surface2O4Dispersion liquid, NiFe2O4The dosage of dispersion liquid is 25 μ L, and accurately rutin and Quercetin progress can be detected simultaneously, reduces the process complexity to rutin and Quercetin detection, reduces cost；And its reproducibility is good, relatively low by the interference effect degree of the impurity such as common metal ion and 200 times of glucose, glycine, citric acid and arginine；And the electrode can also be applied to detect, and detection method is simple rutin in the fruit of Cherokee rose, safflower, the sophora bud and Quercetin progress simultaneously, easily operated.
Description
Technical field
The present invention relates to electrochemical analysis techniques field, especially a kind of electrochemistry based on magnetic Nano NiFe2O4 passes
The preparation method and application of sensor.
Background technology
Flavonoid substances rutin and Quercetin widely exist in Chinese medicine and have in the plant of healthcare function, they join
With the structure of capillary wall, and the permeability and brittleness of blood vessel can be lowered, there is anti-inflammatory, anti-oxidant, antitumor, anti-blood
Platelet aggregation, antiallergy, antiviral, anti-melancholy, anti-ambition hypertrophy, decompression and neuroprotection.But if certain contain
Tablet and the soft capsule storage for having rutin are improper, and perhaps Quercetin is appeared in the hydrolysate of rutin.Sugar as rutin
Base, Quercetin often coexist with rutin.It is often found to collectively reside in Chinese herbal medicine, such as the fruit of Cherokee rose, safflower, the sophora bud etc..
The analysis method detected at present to Quercetin in plant and rutin mainly have spectroscopic methodology, chromatography, spectrophotometry,
Electrochemical process etc..Simple with equipment using detection while electrochemical process progress rutin and Quercetin, detection cycle is short, operation
The advantages that easy, thus with broader practice prospect.Since traditional Electrochemical Detection is to use conventional glass-carbon electrode,
And the oxidizing potential of rutin and Quercetin on conventional glass-carbon electrode is close, the oxidation peak of rutin and Quercetin is overlapped, and is made
It measures and is difficult to while electrochemical method is obtained to rutin and Quercetin, cause to rutin and Quercetin characterization processes complexity,
Testing cost is larger, further result in containing the true and false of rutin and quercitrin extract plant differentiate and quartile length accuracy compared with
It is low；And it is also disclosed in the prior art without any document using NiFe2O4Dispersion liquid carries out reed after carrying out glass-carbon electrode modification
The detection of fourth and Quercetin.
Invention content
In order to solve the above technical problems existing in the prior art, the present invention provides a kind of based on magnetic Nano NiFe2O4
Electrochemical sensor electrode and its preparation method and application.
It is achieved particular by following technical scheme：
One kind is based on magnetic Nano NiFe2O4Electrochemical sensor electrode, by glass-carbon electrode and NiFe2O4Dispersion liquid
Composition, wherein, electrode structure is to coat layer of Ni Fe in glassy carbon electrode surface2O4Dispersion liquid, NiFe2O4The dosage of dispersion liquid is
2-5μL。
The present invention also provides based on magnetic Nano NiFe2O4Electrochemical sensor electrode preparation method, including following
Step：
(1) by FeCl2Solution and NiCl2Solution is (0.9-1.1) according to molar ratio：(2.4-2.6) is uniformly mixed,
Mixed liquor is obtained, then adds in water and glycerine thereto, and pass it through 60-70 DEG C of water bath processing 20-30min, then is added thereto
Enter mix emulsion fluid, continue stir process 50-65min, add the stirring of boracic liquid, then lead at being 60-70 DEG C in bath temperature
Enter nitrogen, and by its reflow treatment 50-65min, be filtered, washed, dry to obtain NiFe2O4, then by NiFe2O4It is mixed with distilled water
Afterwards, it is handled using ultrasonic disperse, mixing ratio is so that the NiFe obtained2O4A concentration of 2-5mg/ml of dispersion liquid, for use；
(2) above-mentioned NiFe is taken2O4Dispersion liquid 2-5 μ L, and by the surface of its drop coating to glass-carbon electrode, then place it in infrared
It is dried under lamp up to magnetic Nano NiFe2O4Modified electrode.
The addition of the addition water and glycerine, wherein water is FeCl21-3 times of solution；The addition of glycerine is
FeCl20.3-0.5 times of solution.
The addition of the mixed emulsion is 1-3 times of glycerine.
The addition of the boracic liquid is 0.7-1 times of glycerine.
The mix emulsion fluid is the mixing of lauryl sodium sulfate, n-amyl alcohol, normal heptane, tbp same-size ratio
Liquid.
The boracic liquid is potassium borohydride, the mixed liquor of n-amyl alcohol, normal heptane same-size ratio.
The present invention also provides be prepared into based on the electrochemical sensor electrode of magnetic Nano NiFe2O4 based on magnetism
Application after the electrochemical sensor of nano-Ni/Fe 2O4 in rutin and Quercetin is measured.
It is above-mentioned to be based on magnetic Nano NiFe2O4Application of the electrochemical sensor in rutin and Quercetin is measured application
Method includes the following steps：
(1) by magnetic Nano NiFe2O4For modified electrode as working electrode, saturated calomel electrode makees reference electrode, platinum filament electricity
Make, to electrode, to obtain electrochemical sensor in pole；
(2) electrochemical sensor that step 1) obtains is placed in the phosphate buffer that pH value is 3-6, is lied prostrate using cycle
Peace method scan, control voltage be 0.1-0.8V, sweep speed be 50 mV/s, scanning until display curve stabilization after, then by its
It is placed in the solution of rutin and Quercetin, and open circuit enrichment 30-120s is carried out to it, stand 2-5s, and be 0.1- in current potential
Differential pulse voltammetry analysis, differential pulse voltammetry analyst coverage 0.1-0.8V, from 0.1V to 0.8V are carried out in the section of 0.8V
Current potential increase as 0.004V, amplitude：0.05V, pulse width：0.2s, sampling width：0.02s, pulse period：0.5s is obtained
The electrochemical sensor is in rutin a concentration of 2.0 × 10- 9- 1.0 × 10- 5Curve and quercetin concentration in the range of mol/L are
5.0×10 - 9- 5.0 × 10- 4Curve in the range of mol/L, and then measure rutin and Quercetin；
(3) in above-mentioned steps 2) it measures and completes and then by magnetic Nano NiFe2O4Modified electrode is placed in the phosphorus that pH is 5.0
In hydrochlorate buffer solution, scan to the electrochemical response of rutin and Quercetin and disappear to 1.2V potential region cyclic voltammetries -0.2
It loses, you can update electrode surface, using NiFe2O4After dispersion liquid modified electrode, magnetic Nano NiFe is obtained2O4Modified electrode, and
It places it in and preserves at room temperature, that is, complete magnetic Nano NiFe2O4Application of the modified electrode in rutin and Quercetin is measured.
The ultrasound used in the present invention, frequency 20-200kHz.
Above-mentioned use based on magnetic Nano NiFe2O4Electrochemical sensor electrode be prepared into based on magnetic Nano
NiFe2O4Electrochemical sensor after in the fruit of Cherokee rose is detected the application process of rutin and quercetin content,
(1) it weighs fruit of Cherokee rose dry product 100g to pulverize, and crossed the sieve of 20 mesh, obtains powder, weighed accurately
It states powder 1g to be placed in container, and 20g absolute ethyl alcohols ultrasonic extraction processing 45min is added in into container, filter to obtain extracting solution, then
Extracting solution in volumetric flask is settled to 50mL with absolute ethyl alcohol, shakes up, obtains testing sample solution；
(2) the testing sample solution 0.5ml that step 1) is taken to obtain, in 100mL volumetric flasks, uses B-R buffer solution constant volumes
50ml is diluted to, then using magnetic Nano NiFe2O4For modified electrode as working electrode, saturated calomel electrode makees reference electrode, platinum
Silk electrode is made to electrode, obtains electrochemical sensor and carries out open circuit enrichment 30-120s, stands 2-5s, and is 0.1- in current potential
Differential pulse voltammetry analysis, differential pulse voltammetry analyst coverage 0.1-0.8V, from 0.1V to 0.8V are carried out in the section of 0.8V
Current potential increase as 0.004V, amplitude：0.05V, pulse width：0.2s, sampling width：0.02s, pulse period：0.5s, you can
Complete the detection of rutin and quercetin content in the fruit of Cherokee rose.
The present invention is by indicating the rutin in the fruit of Cherokee rose and the testing result of quercetin content with ultraviolet spectrophotometry
Value is compared, and error is smaller；By 1.0 × 10-6mol/L rutins and Quercetin mixed standard solution METHOD FOR CONTINUOUS DETERMINATION 8 times, difference arteries and veins
The relative standard deviation (RSD) for rushing volt-ampere oxidation peak peak height is respectively 3.48% and 4.79%, and then can effectively distinguish
Rutin and Quercetin, and then reach the detection to rutin and Quercetin；And its reproducibility is good；
Furthermore invention is also handled by recovery testu, and the rate of being recycled has reached 97.8%~101.6%, and then
As it can be seen that the application of electrode is higher in the accuracy that rutin and Quercetin detect.
And the present invention also tests error influence factor, when error is ± 5%, Na+、K+、Fe3+、Cu2+、
A13+、Mg2+、Ca2+Etc. common metal ions and 200 times of glucose, glycine, citric acid and arginine etc. to rutin and
The measure of Quercetin solution does not interfere, further improves the accuracy to rutin and quercetin content detection, drop
Low detection difficulty.
It is prepared for magnetic Nano NiFe2O4, using magnetic Nano NiFe2O4Ultrasonic disperse takes NiFe in distilled water2O4Point
Dispersion liquid drop coating is to the surface of processed good glass-carbon electrode, then is placed under infrared lamp and dries up to magnetic Nano NiFe2O4Modification electricity
Pole, and three-electrode system is formed with saturated calomel electrode, platinum electrode, provide electricity that is a kind of while measuring rutin and Quercetin
Chemical method.Experiments verify that the three-electrode system has higher catalytic activity, the sensitivity of detection to rutin and Quercetin
Height, the overpotential of oxidation reaction is low, and selectivity is good, can realize to being measured while rutin and Quercetin, be a kind of high stable
Property, high sensitivity and highly selective detecting electrode, and its preparation process is simple, it is of low cost.
Specific embodiment
It is limited with reference to specific embodiment technical scheme of the present invention is further, but claimed
Range is not only limited to made description.
Embodiment 1
One kind is based on magnetic Nano NiFe2O4Electrochemical sensor electrode, by glass-carbon electrode and NiFe2O4Dispersion liquid
Composition, wherein, electrode structure is to coat layer of Ni Fe in glassy carbon electrode surface2O4Dispersion liquid, NiFe2O4The dosage of dispersion liquid is
2μL。
It should be based on magnetic Nano NiFe2O4Electrochemical sensor electrode preparation method,
(1) by FeCl2Solution and NiCl2Solution is 0.9 according to molar ratio：2.6 are uniformly mixed, and obtain mixed liquor, then
Water and glycerine are added in thereto, and passes it through 70 DEG C of water bath processing 30min, then add in mix emulsion fluid thereto, continue to stir
Processing 65min is mixed, adds the stirring of boracic liquid, then in bath temperature to be passed through nitrogen at 70 DEG C, and by its reflow treatment
65min is filtered, washed, dries to obtain NiFe2O4, then by NiFe2O4It after being mixed with distilled water, is handled, mixed using ultrasonic disperse
Than for so that the NiFe obtained2O4A concentration of 5mg/ml of dispersion liquid, for use；
(2) above-mentioned NiFe is taken2O42 μ L of dispersion liquid, and by the surface of its drop coating to glass-carbon electrode, then place it in infrared lamp
Under dry up to magnetic Nano NiFe2O4Modified electrode.
The addition of the addition water and glycerine, wherein water is FeCl21 times of solution；The addition of glycerine is FeCl2
0.3 times of solution.
The addition of the mixed emulsion is 1 times of glycerine.
The addition of the boracic liquid is 0.7 times of glycerine.
The mix emulsion fluid is the mixing of lauryl sodium sulfate, n-amyl alcohol, normal heptane, tbp same-size ratio
Liquid.
The boracic liquid is potassium borohydride, the mixed liquor of n-amyl alcohol, normal heptane same-size ratio.
Embodiment 2
One kind is based on magnetic Nano NiFe2O4Electrochemical sensor electrode, by glass-carbon electrode and NiFe2O4Dispersion liquid
Composition, wherein, electrode structure is to coat layer of Ni Fe in glassy carbon electrode surface2O4Dispersion liquid, NiFe2O4The dosage of dispersion liquid is
5μL。
It should be based on magnetic Nano NiFe2O4Electrochemical sensor electrode preparation method,
(1) by FeCl2Solution and NiCl2Solution is 1.1 according to molar ratio：2.4 are uniformly mixed, and obtain mixed liquor, then
Water and glycerine are added in thereto, and passes it through 60 DEG C of water bath processing 20min, then add in mix emulsion fluid thereto, continue to stir
Processing 50min is mixed, adds the stirring of boracic liquid, then in bath temperature to be passed through nitrogen at 60 DEG C, and by its reflow treatment
50min is filtered, washed, dries to obtain NiFe2O4, then by NiFe2O4It after being mixed with distilled water, is handled, mixed using ultrasonic disperse
Than for so that the NiFe obtained2O4A concentration of 2mg/ml of dispersion liquid, for use；
(2) above-mentioned NiFe is taken2O45 μ L of dispersion liquid, and by the surface of its drop coating to glass-carbon electrode, then place it in infrared lamp
Under dry up to magnetic Nano NiFe2O4Modified electrode.
The addition of the addition water and glycerine, wherein water is FeCl23 times of solution；The addition of glycerine is FeCl2
0.5 times of solution.
The addition of the mixed emulsion is 3 times of glycerine.
The addition of the boracic liquid is 1 times of glycerine.
The mix emulsion fluid is the mixing of lauryl sodium sulfate, n-amyl alcohol, normal heptane, tbp same-size ratio
Liquid.
The boracic liquid is potassium borohydride, the mixed liquor of n-amyl alcohol, normal heptane same-size ratio.
Embodiment 3
One kind is based on magnetic Nano NiFe2O4Electrochemical sensor electrode, by glass-carbon electrode and NiFe2O4Dispersion liquid
Composition, wherein, electrode structure is to coat layer of Ni Fe in glassy carbon electrode surface2O4Dispersion liquid, NiFe2O4The dosage of dispersion liquid is
3μL。
It should be based on magnetic Nano NiFe2O4Electrochemical sensor electrode preparation method,
(1) by FeCl2Solution and NiCl2Solution is 1 according to molar ratio：2.5 are uniformly mixed, acquisition mixed liquor, then to
Water and glycerine are wherein added in, and passes it through 65 DEG C of water bath processing 25min, then add in mix emulsion fluid thereto, continues to stir
60min is handled, adds the stirring of boracic liquid, then in bath temperature to be passed through nitrogen at 65 DEG C, and by its reflow treatment 60min,
It is filtered, washed, dries to obtain NiFe2O4, then by NiFe2O4It after being mixed with distilled water, is handled using ultrasonic disperse, mixing ratio is makes
The NiFe that must be obtained2O4A concentration of 4mg/ml of dispersion liquid, for use；
(2) above-mentioned NiFe is taken2O43 μ L of dispersion liquid, and by the surface of its drop coating to glass-carbon electrode, then place it in infrared lamp
Under dry up to magnetic Nano NiFe2O4Modified electrode.
The addition of the addition water and glycerine, wherein water is FeCl22 times of solution；The addition of glycerine is FeCl2
0.4 times of solution.
The addition of the mixed emulsion is 2 times of glycerine.
The addition of the boracic liquid is 0.8 times of glycerine.
The mix emulsion fluid is the mixing of lauryl sodium sulfate, n-amyl alcohol, normal heptane, tbp same-size ratio
Liquid.
The boracic liquid is potassium borohydride, the mixed liquor of n-amyl alcohol, normal heptane same-size ratio.
Embodiment 4
Embodiment 1 is obtained to be based on magnetic Nano NiFe2O4Electrochemical sensor be prepared into electrode based on magnetic Nano
NiFe2O4Electrochemical sensor after application in detection rutin and quercetin content, specific application process is：(1) by magnetic
Property nano-Ni/Fe2O4For modified electrode as working electrode, saturated calomel electrode makees reference electrode, and platinum electrode is made, to electrode, to obtain
Electrochemical sensor；
(2) electrochemical sensor that step 1) obtains is placed in the phosphate buffer that pH value is 3, using cyclic voltammetric
Method scans, and control voltage is 0.1-0.8V, and sweep speed is 50 mV/s, and scanning is after the curve of display is stablized, then is put
In the solution of rutin and Quercetin, and open circuit enrichment 30s is carried out to it, stand 2s, and in the section that current potential is 0.1-0.8V
Interior progress differential pulse voltammetry analysis, differential pulse voltammetry analyst coverage 0.1-0.8V, the current potential from 0.1V to 0.8V increase
For 0.004V, amplitude：0.05V, pulse width：0.2s, sampling width：0.02s, pulse period：0.5s show that the electrochemistry passes
Sensor is in rutin a concentration of 2.0 × 10- 9- 1.0 × 10- 5Curve and quercetin concentration in the range of mol/L are 5.0 × 10- 9- 5.0 × 10- 4Curve in the range of mol/L, and then measure rutin and Quercetin；
(3) in above-mentioned steps 2) it measures and completes and then by magnetic Nano NiFe2O4Modified electrode is placed in the phosphorus that pH is 5.0
In hydrochlorate buffer solution, scan to the electrochemical response of rutin and Quercetin and disappear to 1.2V potential region cyclic voltammetries -0.2
It loses, you can update electrode surface, using NiFe2O4After dispersion liquid modified electrode, magnetic Nano NiFe is obtained2O4Modified electrode, and
It places it in and preserves at room temperature, that is, complete based on magnetic Nano NiFe2O4Electrochemical sensor electrode measuring rutin and Mongolian oak
Application in Pi Su.
Embodiment 5
Embodiment 2 is obtained to be based on magnetic Nano NiFe2O4Electrochemical sensor electrode received based on magnetism being prepared into
Rice NiFe2O4Electrochemical sensor after application in detection rutin and quercetin content, specific application process is：(1) will
Magnetic Nano NiFe2O4For modified electrode as working electrode, saturated calomel electrode makees reference electrode, and platinum electrode is made to electrode, obtained
Obtain electrochemical sensor；
(2) electrochemical sensor that step (1) obtains is placed in the phosphate buffer that pH value is 6, is lied prostrate using cycle
Peace method scan, control voltage be 0.1-0.8V, sweep speed be 50 mV/s, scanning until display curve stabilization after, then by its
It is placed in the solution of rutin and Quercetin, and open circuit enrichment 120s is carried out to it, stand 5s, and in the area that current potential is 0.1-0.8V
Interior progress differential pulse voltammetry analysis, differential pulse voltammetry analyst coverage 0.1-0.8V, the current potential from 0.1V to 0.8V increase
Add as 0.004V, amplitude：0.05V, pulse width：0.2s, sampling width：0.02s, pulse period：0.5s obtains the electrochemistry
Sensor is in rutin a concentration of 2.0 × 10- 9- 1.0 × 10- 5Curve and quercetin concentration in the range of mol/L are 5.0 × 10- 9- 5.0 × 10- 4Curve in the range of mol/L, and then measure rutin and Quercetin；
(3) it measures and completes and then by magnetic Nano NiFe in above-mentioned steps (2)2O4It is 5.0 that modified electrode, which is placed in pH,
In phosphate buffer solution, the electrochemical response to rutin and Quercetin is scanned to 1.2V potential region cyclic voltammetries -0.2
It disappears, you can update electrode surface, using NiFe2O4After dispersion liquid modified electrode, magnetic Nano NiFe is obtained2O4Modified electrode,
And place it in and preserve at room temperature, that is, it completes based on magnetic Nano NiFe2O4Electrochemical sensor electrode measure rutin and
Application in Quercetin.
Embodiment 6
Embodiment 3 is obtained to be based on magnetic Nano NiFe2O4Electrochemical sensor electrode received based on magnetism being prepared into
Rice NiFe2O4Electrochemical sensor after application in detection rutin and quercetin content, specific application process is：(1) will
Magnetic Nano NiFe2O4For modified electrode as working electrode, saturated calomel electrode makees reference electrode, and platinum electrode is made to electrode, obtained
Obtain electrochemical sensor；
(2) electrochemical sensor that step (1) obtains is placed in the phosphate buffer that pH value is 5, is lied prostrate using cycle
Peace method scan, control voltage be 0.1-0.8V, sweep speed be 50 mV/s, scanning until display curve stabilization after, then by its
It is placed in the solution of rutin and Quercetin, and open circuit enrichment 90s is carried out to it, stand 3s, and in the area that current potential is 0.1-0.8V
Interior progress differential pulse voltammetry analysis, differential pulse voltammetry analyst coverage 0.1-0.8V, the current potential from 0.1V to 0.8V increase
Add as 0.004V, amplitude：0.05V, pulse width：0.2s, sampling width：0.02s, pulse period：0.5s obtains the electrochemistry
Sensor is in rutin a concentration of 2.0 × 10- 9- 1.0 × 10- 5Curve and quercetin concentration in the range of mol/L are 5.0 × 10- 9- 5.0 × 10- 4Curve in the range of mol/L, and then measure rutin and Quercetin；
(3) it measures and completes and then by magnetic Nano NiFe in above-mentioned steps (2)2O4It is 5.0 that modified electrode, which is placed in pH,
In phosphate buffer solution, the electrochemical response to rutin and Quercetin is scanned to 1.2V potential region cyclic voltammetries -0.2
It disappears, you can update electrode surface, using NiFe2O4After dispersion liquid modified electrode, magnetic Nano NiFe is obtained2O4Modified electrode,
And place it in and preserve at room temperature, that is, it completes based on magnetic Nano NiFe2O4Electrochemical sensor electrode measure rutin and
Application in Quercetin.
Embodiment 7
Embodiment 1 prepare based on magnetic Nano NiFe2O4Electrochemical sensor electrode received based on magnetism being prepared into
Rice NiFe2O4Electrochemical sensor after in the fruit of Cherokee rose is detected the application process of rutin and quercetin content,
(1) it weighs fruit of Cherokee rose dry product 100g to pulverize, and crossed the sieve of 20 mesh, obtains powder, weighed accurately
It states powder 1g to be placed in container, and 20g absolute ethyl alcohols ultrasonic extraction processing 45min is added in into container, filter to obtain extracting solution, then
Extracting solution in volumetric flask is settled to 50mL with absolute ethyl alcohol, shakes up, obtains testing sample solution；
(2) the testing sample solution 0.5ml that step (1) is taken to obtain, in 100mL volumetric flasks, uses B-R buffer solution constant volumes
50ml is diluted to, then using magnetic Nano NiFe2O4For modified electrode as working electrode, saturated calomel electrode makees reference electrode, platinum
Silk electrode is made to electrode, obtains electrochemical sensor and carries out open circuit enrichment 50s, stands 4s, and in the area that current potential is 0.1-0.8V
Interior progress differential pulse voltammetry analysis, differential pulse voltammetry analyst coverage 0.1-0.8V, the current potential from 0.1V to 0.8V increase
Add as 0.004V, amplitude：0.05V, pulse width：0.2s, sampling width：0.02s, pulse period：0.5s, you can complete golden cherry
The detection of rutin and quercetin content in son.
Embodiment 8
Embodiment 2 prepare based on magnetic Nano NiFe2O4Electrochemical sensor be prepared into electrode based on magnetic Nano
NiFe2O4Electrochemical sensor after in safflower is detected the application process of rutin and quercetin content,
(1) it weighs safflower dry product 100g to pulverize, and crossed the sieve of 20 mesh, obtains powder, it is above-mentioned accurately weighing
Powder 1g is placed in container, and 20g absolute ethyl alcohols ultrasonic extraction processing 45min is added in into container, filters to obtain extracting solution, then use
Extracting solution is settled to 50mL by absolute ethyl alcohol in volumetric flask, is shaken up, and obtains testing sample solution；
(2) the testing sample solution 0.5ml that step (1) is taken to obtain, in 100mL volumetric flasks, uses B-R buffer solution constant volumes
50ml is diluted to, then using magnetic Nano NiFe2O4For modified electrode as working electrode, saturated calomel electrode makees reference electrode, platinum
Silk electrode is made to electrode, obtains electrochemical sensor and carries out open circuit enrichment 60s, stands 3s, and in the area that current potential is 0.1-0.8V
Interior progress differential pulse voltammetry analysis, differential pulse voltammetry analyst coverage 0.1-0.8V, the current potential from 0.1V to 0.8V increase
Add as 0.004V, amplitude：0.05V, pulse width：0.2s, sampling width：0.02s, pulse period：0.5s, you can complete golden cherry
The detection of rutin and quercetin content in son.
Embodiment 9
Embodiment 3 prepare based on magnetic Nano NiFe2O4Electrochemical sensor electrode received based on magnetism being prepared into
Rice NiFe2O4Electrochemical sensor after in the sophora bud is detected the application process of rutin and quercetin content,
(1) it weighs sophora bud dry product 100g to pulverize, and crossed the sieve of 20 mesh, obtains powder, it is above-mentioned accurately weighing
Powder 1g is placed in container, and 20g absolute ethyl alcohols ultrasonic extraction processing 45min is added in into container, filters to obtain extracting solution, then use
Extracting solution is settled to 50mL by absolute ethyl alcohol in volumetric flask, is shaken up, and obtains testing sample solution；
(2) the testing sample solution 0.5ml that step (1) is taken to obtain, in 100mL volumetric flasks, uses B-R buffer solution constant volumes
50ml is diluted to, then using magnetic Nano NiFe2O4For modified electrode as working electrode, saturated calomel electrode makees reference electrode, platinum
Silk electrode is made to electrode, obtains electrochemical sensor and carries out open circuit enrichment 70s, stands 5s, and in the area that current potential is 0.1-0.8V
Interior progress differential pulse voltammetry analysis, differential pulse voltammetry analyst coverage 0.1-0.8V, the current potential from 0.1V to 0.8V increase
Add as 0.004V, amplitude：0.05V, pulse width：0.2s, sampling width：0.02s, pulse period：0.5s, you can complete golden cherry
The detection of rutin and quercetin content in son.
Claims (6)
1. one kind is based on magnetic Nano NiFe2O4Electrochemical sensor determination of electrode rutin and the method for Quercetin, feature
It is, the electrochemical sensor is by glass-carbon electrode and NiFe2O4Dispersion liquid forms, wherein, electrode structure is in glass-carbon electrode table
Face coating layer of Ni Fe2O4Dispersion liquid, NiFe2O4The dosage of dispersion liquid is 2-5 μ L；
It is above-mentioned based on magnetic Nano NiFe2O4Electrochemical sensor electrode preparation method, include the following steps：
(1) by FeCl2Solution and NiCl2Solution is 0.9-1.1 according to molar ratio：2.4-2.6 is uniformly mixed, and is mixed
Liquid, then water and glycerine are added in thereto, and pass it through 60-70 DEG C of water bath processing 20-30min, then add in mixing breast thereto
Change liquid, continue stir process 50-65min, add the stirring of boracic liquid, then nitrogen is passed through at being 60-70 DEG C in bath temperature, and
By its reflow treatment 50-65min, it is filtered, washed, dries to obtain NiFe2O4, then by NiFe2O4After being mixed with distilled water, using super
Sound decentralized processing, mixing ratio are so that the NiFe obtained2O4A concentration of 2-5mg/ml of dispersion liquid, for use；The addition water and
The addition of glycerine, wherein water is FeCl21-3 times of solution；The addition of glycerine is FeCl20.3-0.5 times of solution；
(2) above-mentioned NiFe is taken2O4Dispersion liquid 2-5 μ L, and by the surface of its drop coating to glass-carbon electrode, then place it under infrared lamp
It dries up to magnetic Nano NiFe2O4Modified electrode；
The method for measuring rutin and Quercetin, includes the following steps：
(1) by magnetic Nano NiFe2O4For modified electrode as working electrode, saturated calomel electrode makees reference electrode, and platinum electrode is made
To electrode, electrochemical sensor is obtained；
(2) electrochemical sensor that step (1) obtains is placed in the phosphate buffer that pH value is 3-6, using cyclic voltammetric
Method scans, and control voltage is 0.1-0.8V, sweep speed 50mV/s, and scanning is after the curve of display is stablized, then is put
In the solution of rutin and Quercetin, and open circuit enrichment 30-120s is carried out to it, stand 2-5s, and be 0.1-0.8V in current potential
Section in carry out differential pulse voltammetry analysis, differential pulse voltammetry analyst coverage be 0.1-0.8V, the electricity from 0.1V to 0.8V
Position increases as 0.004V, amplitude：0.05V, pulse width：0.2s, sampling width：0.02s, pulse period：0.5s obtains the electricity
Chemical sensor is in rutin a concentration of 2.0 × 10- 9- 1.0 × 10- 5Curve and quercetin concentration in the range of mol/L for 5.0 ×
10- 9- 5.0 × 10- 4Curve in the range of mol/L, and then measure rutin and Quercetin；
(3) it measures and completes and then by magnetic Nano NiFe in above-mentioned steps (2)2O4Modified electrode is placed in the phosphoric acid that pH is 5.0
In salt buffer solution, scan to the electrochemical response of rutin and Quercetin and disappear to 1.2V potential region cyclic voltammetries -0.2
It loses, you can update electrode surface, using NiFe2O4After dispersion liquid modified electrode, magnetic Nano NiFe is obtained2O4Modified electrode, and
It places it in and preserves at room temperature, that is, complete magnetic Nano NiFe2O4Application of the modified electrode in rutin and Quercetin is measured.
2. it is based on magnetic Nano NiFe as described in claim 12O4Electrochemical sensor determination of electrode rutin and Quercetin
Method, it is characterised in that：The addition of the mix emulsion fluid is 1-3 times of glycerine.
3. it is based on magnetic Nano NiFe as described in claim 12O4Electrochemical sensor determination of electrode rutin and Quercetin
Method, it is characterised in that：The addition of the boracic liquid is 0.7-1 times of glycerine.
4. it is based on magnetic Nano NiFe as claimed in claim 1 or 22O4Electrochemical sensor determination of electrode rutin and Mongolian oak
The method of Pi Su, it is characterised in that：The mix emulsion fluid is lauryl sodium sulfate, n-amyl alcohol, normal heptane, tricresyl phosphate fourth
The mixed liquor of fat same-size ratio.
5. as described in claim 1 or 3 based on magnetic Nano NiFe2O4Electrochemical sensor determination of electrode rutin and Mongolian oak
The method of Pi Su, it is characterised in that：The boracic liquid is potassium borohydride, the mixed liquor of n-amyl alcohol, normal heptane same-size ratio.
6. with the method for the content of rutin and Quercetin in claim 1 the method detection fruit of Cherokee rose, it is characterised in that：Including
Following steps：
(1) it weighs fruit of Cherokee rose dry product 100g to pulverize, and crossed the sieve of 20 mesh, obtains powder, then accurately weigh above-mentioned powder
Last 1g is placed in container, and 20g absolute ethyl alcohols ultrasonic extractions processing 45min is added in into container, filters to obtain extracting solution, then with nothing
Extracting solution is settled to 50mL by water-ethanol in volumetric flask, is shaken up, and obtains testing sample solution；
(2) the testing sample solution 0.5ml that step (1) is taken to obtain in 100mL volumetric flasks, is diluted using B-R buffer solutions constant volume
To 50ml, then using magnetic Nano NiFe2O4For modified electrode as working electrode, saturated calomel electrode makees reference electrode, platinum filament electricity
Pole is made to electrode, obtains electrochemical sensor and carries out open circuit enrichment 30-120s, stands 2-5s, and is 0.1-0.8V's in current potential
In section carry out differential pulse voltammetry analysis, differential pulse voltammetry analyst coverage be 0.1-0.8V, the current potential from 0.1V to 0.8V
Increase as 0.004V, amplitude：0.05V, pulse width：0.2s, sampling width：0.02s, pulse period：0.5s, you can complete gold
The detection of rutin and quercetin content in cherry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510270421.0A CN104914147B (en) | 2015-05-25 | 2015-05-25 | One kind is based on magnetic Nano NiFe2O4Electrochemical sensor preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510270421.0A CN104914147B (en) | 2015-05-25 | 2015-05-25 | One kind is based on magnetic Nano NiFe2O4Electrochemical sensor preparation method and application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104914147A CN104914147A (en) | 2015-09-16 |
| CN104914147B true CN104914147B (en) | 2018-07-10 |
Family
ID=54083395
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510270421.0A Active CN104914147B (en) | 2015-05-25 | 2015-05-25 | One kind is based on magnetic Nano NiFe2O4Electrochemical sensor preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104914147B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106198665B (en) * | 2016-06-27 | 2019-01-29 | 衡阳师范学院 | A kind of electrochemical method of levodopa amine quantitative detection |
| CN106124593B (en) * | 2016-08-12 | 2019-02-05 | 浙江大学 | It is a kind of for the composite material modified electrode of measure glucose concentration and application |
| CN114324518B (en) * | 2021-12-09 | 2024-02-06 | 北京市农林科学院智能装备技术研究中心 | Microelectrode, detection method of rutin and quercetin and application |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100412538C (en) * | 2005-11-10 | 2008-08-20 | 上海师范大学 | A test bar and its preparing process, and method for synchronous detecting rutin and vitamin C in medicine with the same testing bar |
| CN101581691B (en) * | 2009-06-26 | 2012-08-29 | 上海大学 | Preparation method of modified glassy carbon electrode as glucose sensor and application thereof |
| CN102288669B (en) * | 2011-05-04 | 2013-06-26 | 青岛大学 | Electrochemical method based on graphene-modified electrode for simultaneous determination of rutin and quercetin |
-
2015
- 2015-05-25 CN CN201510270421.0A patent/CN104914147B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104914147A (en) | 2015-09-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104914147B (en) | One kind is based on magnetic Nano NiFe2O4Electrochemical sensor preparation method and application | |
| CN103604849B (en) | Electrochemical sensor capable of simultaneously detecting dopamine, ascorbic acid and uric acid | |
| CN106645450B (en) | The quality determining method of novel biochemical particles | |
| CN109254041B (en) | Electrochemical detection method for capsaicin in hot pepper | |
| CN104569170A (en) | Method for detecting ginkgo leaf extract and diphyridamole injection preparation | |
| CN104714037A (en) | Method for testing content of monosaccharide in polysaccharide in pear peel tissue | |
| CN103808835B (en) | The method of 10 kinds of chemical composition contents in HPLC-DAD method Simultaneously test Siwu Tang decoction | |
| CN107340348A (en) | A kind of method for building up of Bletilla striata medicinal materials HPLC finger-prints | |
| Alarfaj | Square-wave adsorptive stripping voltammetric determination of antihypertensive agent telmisartan in tablets and its application to human plasma | |
| CN105223260B (en) | Electrochemical sensor of trace quick detection butyl p-hydroxybenzoate and preparation method thereof | |
| CN107421975B (en) | The detection method of glycerol content in a kind of injection | |
| Zhang et al. | Electrochemical determination of synephrine by using nafion/UiO-66/graphene-modified screen-printed carbon electrode | |
| CN106226423A (en) | Pyrazine and the method for pyridines material in a kind of separation determination saliva | |
| CN106950309B (en) | The not method of quality control of the Radix Angelicae Sinensis of same amount ratio and safflower medicine pair | |
| Guo et al. | Enhanced electrochemical determination of quercetin in a choline chloride-based ionic liquid | |
| CN109738544A (en) | The detection for integrating dissolution rate of terpene lactones and flavonoid glycoside ingredient and verification method in a kind of Bilobanoate piece | |
| CN106404868A (en) | Microelectrode biosensor for online detection of GAs (gibberellins) in living plant and application of microelectrode biosensor | |
| Cen et al. | Development of a fast method for Fructus aurantii identification by electrochemical fingerprint | |
| CN103575820B (en) | The analysis method of 5 kinds of flavonoid glycosides and application in pharmacokinetics thereof in blood plasma | |
| CN108426957A (en) | A method of it is surveyed using one and comments method to detect plurality of active ingredients content in hawthorne leaf P.E more | |
| CN103353499A (en) | Method for simultaneously measuring gulonic acid, gulonic acid methyl ester and vitamin C through constant current performance liquid chromatography | |
| CN104914174B (en) | A kind of content assaying method of injection ginkgo diterpenoid-lactone | |
| CN107224753A (en) | A kind of method of utilization Magnetic solid phases extraction sorbing material enrichment detection camptothecine | |
| CN103149207A (en) | Nano-gold-based method for visually and rapidly detecting antibiotics in milk | |
| Ling-Fen et al. | In vivo detection of L-tryptophan in cucumbers using poly (9-Aminoacridine) film modified pencil graphite electrode |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |