CN107505374A - Detect the method for content of luteolin and its chemically modified electrode of use and preparation in Radix Lamiophlomidis Rotatae capsule - Google Patents
Detect the method for content of luteolin and its chemically modified electrode of use and preparation in Radix Lamiophlomidis Rotatae capsule Download PDFInfo
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Abstract
The invention discloses the method for content of luteolin and its chemically modified electrode of use and preparation in a kind of detection Radix Lamiophlomidis Rotatae capsule, it is the relation of peak point current and its gradient concentration that cyanidenon is detected by Differential Pulse Voltammetry, establish standard curve and then cyanidenon standard liquid is added in the sample solution prepared in advance, carry out rate of recovery experiment.It is by gold nanometer cage to detect the chemically modified electrode used（AuNCs）Uniform drop coating grinds the carbon ion liquid electrode uniformly made by a certain percentage to by 1 hexyl pyridine hexafluorophosphate and graphite powder（CILE）Dry in the shade to obtain in surface.The gold nanometer cage modified carbon ionic liquid electrode preparation method of the present invention is simple, and preparation cost is low, and preparation process is environment friendly and pollution-free, and the electrode potential window of preparation is wide, conducts electricity very well.Use it for having the characteristics that in the measure of content of luteolin that high sensitivity, test limit are low, stability is good, favorable reproducibility and strong interference immunity.
Description
Technical field
The invention belongs to electrochemical analysis techniques field, and in particular to content of luteolin in one kind detection Radix Lamiophlomidis Rotatae capsule
Method and its use chemically modified electrode and preparation.
Background technology
Cyanidenon is one kind of flavone compound, and its molecular formula is C15H10O6, dragonhead, capsicum, honeysuckle,
Content is higher in the plants such as chrysanthemum indicum purple perilla, has important pharmacological activity, such as anti-inflammatory, cough-relieving, anti-oxidant, raising immunocompetence
And other effects, and toxic side effect is small, is a kind of more effect medicines.
Mainly there are capillary electrophoresis, AAS and high-efficient liquid phase color to the method for content of luteolin detection at present
The methods of spectrometry, these methods respectively have its advantage and disadvantage, in general with cumbersome, poor sensitivity, expensive equipment, the degree of accuracy
The shortcomings of not high.
Chinese patent literature CN105259225A（Application number 201510700336.3）It is quick to disclose a kind of cyanidenon
Selective enumeration method method and its special electrochemical sensor, the detection method specifically include：1）By Chinese medicine or Chinese patent medicine preparation
Powder is ground into, extracts 12h with absolute ethyl alcohol and stirring, filtering is calmly molten to obtain test liquid；2）Using electrochemical sensor to for trying
Liquid is tested and analyzed, and determines the content of cyanidenon.Wherein electrochemical sensor is that nano composite material N-GR-EDOTM is repaiied
Electrode is adornd, the electrochemical sensor can realize, sensitive, selective enumeration method efficient to cyanidenon, and be successfully applied to Chinese medicine original
Expect the trace detection of content of luteolin in medicine and Chinese patent medicine preparation.This method belongs to electrochemical reducing and prepares N doping graphite
Alkene modified electrode, N-GR-EDOTM aqueous dispersions are deposited into clean GCE surfaces of polishing using cyclic voltammetry, by what is obtained
Modified electrode is repeatedly rinsed with deionized water to remove the monomer of residual.Although this method significant effect, its practical operation
Step is relatively complicated, and has certain contaminated wastewater, therefore provides and a kind of prepare more economical, convenient and environmentally friendly height
Selectivity, the new chemical modified electrode of highly sensitive detection cyanidenon are necessary.
The content of the invention
Present invention aims at solve the above problems, there is provided a kind of method for detecting content of luteolin in Radix Lamiophlomidis Rotatae capsule
And its chemically modified electrode used and preparation.
Realizing the technical scheme of the object of the invention is：A kind of method of content of luteolin in detection Radix Lamiophlomidis Rotatae capsule, tool
There are following steps：
S1：Prepare Radix Lamiophlomidis Rotatae capsule sample solution；
S2：Using chemically modified electrode as working electrode, platinized platinum is auxiliary electrode, and saturated calomel electrode is reference electrode, by showing
The relation of the peak point current and its gradient concentration of poor pulse voltammetry detection cyanidenon, establishes standard curve；
S3：Cyanidenon standard liquid is added in the sample solution of above-mentioned steps S1 preparations, carries out rate of recovery experiment, measure
The rate of recovery.
The preparation process of Radix Lamiophlomidis Rotatae capsule sample solution is as follows described in above-mentioned steps S1：Radix Lamiophlomidis Rotatae capsule is removed into shell
With soaked in absolute ethyl alcohol and flow back, then filter, filtrate produces after being diluted with phosphate buffer afterwards.
The pH of the phosphate buffer is 3.
The concentration of cyanidenon standard liquid described in above-mentioned steps S3 is 1.0 × 10-6mol/L。
Chemically modified electrode described in above-mentioned steps S2 is gold nanometer cage modified carbon ionic liquid electrode（AuNCs/
CILE）.
Above-mentioned gold nanometer cage modified carbon ionic liquid electrode（AuNCs/CILE）Preparation method it is as follows：
1. 1- hexyl pyridine hexafluorophosphates and graphite powder are ground uniformly, carbon ion liquid paste is obtained；
2. inserting in vitreous electricity pole pipe and being compacted 1. carbon ion liquid that step obtains paste, be inserted into copper wire, obtain carbon from
Sub- liquid electrode（CILE）；
3. by gold nanometer cage（AuNCs）2. carbon ion liquid electrode surface that uniform drop coating obtains to step, dries in the shade and produces Jenner
Rice cage modified carbon ionic liquid electrode（AuNCs/CILE）.
Above-mentioned steps 1. described in the weight ratio of 1- hexyl pyridine hexafluorophosphates and the graphite powder be 1: 1~1: 3, it is excellent
Elect 1: 2 as.
The present invention has positive effect：The gold nanometer cage modified carbon ionic liquid electrode preparation method of the present invention is simple,
Preparation cost is low, and preparation process is environment friendly and pollution-free, and the electrode potential window of preparation is wide, conducts electricity very well.Use it for reseda
Have the characteristics that high sensitivity, test limit are low, stability is good, favorable reproducibility and strong interference immunity in the measure of cellulose content.
Brief description of the drawings
Fig. 1 is gold nanometer cage modified carbon ionic liquid electrode prepared by example 1（AuNCs/CILE）Scanning electron microscope (SEM) photograph.
Fig. 2 is that the CILE and AuNCs/CILE of test case 1 detect the cyclic voltammetric response diagram of cyanidenon；Wherein, curve a
AuNCs/CILE is represented, curve b represents CILE.
Fig. 3 detects the cyclic voltammetric response diagram of cyanidenon for AuNCs/CILE under the different scanning speed of test case 2；Its
In, a to j represents 0.02V/s, 0.04V/s, 0.06V/s, 0.08V/s, 0.1V/s, 0.14V/s, 0.18V/s, 0.22V/ respectively
S, 0.26V/s, 0.3V/s sweep speed.
Fig. 4 is the differential pulse volt-ampere superposition that the AuNCs/CILE of test case 3 detects the luteolin solution of various concentrations
Figure；Wherein, a to j represents 0.04,0.08,0.6,0.8,1,2,4,6,8,10 μm of ol/L respectively.
Fig. 5 detects the circulation volt of cyanidenon for AuNCs/CILE in the phosphate buffer of the different pH value of test case 4
Pacify response diagram；Wherein, a to g represents pH value as 2.0,3.0,4.0,5.0,6.0,7.0,8.0 respectively.
Fig. 6 detects the Middle Eocene of cyanidenon for AuNCs/CILE in the phosphate buffer of the different pH value of test case 5.
Fig. 7 is the CILE and AuNCs/CILE of test case 6 AC impedance spectroscopy；Wherein, curve a represents CILE, curve b
Represent AuNCs/CILE.
Embodiment
（Example 1）
This example is gold nanometer cage modified carbon ionic liquid electrode（AuNCs/CILE）Making：
1. accurately weighing 1.20g 1- hexyl pyridine hexafluorophosphates and 2.40g graphite powder, it is then placed in agate mortar and grinds
Mill is uniform, obtains carbon ion liquid paste；
2. selection length be 2.5cm, a diameter of 4mm vitreous electricity pole pipe and clean drying, be then filled with 1. carbon that step obtains
Ionic Liquid Paste is simultaneously firmly compacted, and is then inserted into a copper wire as wire, is obtained carbon ion liquid electrode（CILE）.
3. the carbon ion liquid electrode 2. obtained to step characterizes, it is determined for compliance with after using standard, using rubbing method
By gold nanometer cage（AuNCs）Uniform drop coating is to carbon ion liquid electrode surface, after the 2.5h that dries in the shade, obtain gold nanometer cage modified carbon from
Sub- liquid electrode（AuNCs/CILE）.
Gold nanometer cage modified carbon ionic liquid electrode made from this example（AuNCs/CILE）Scanning electron microscope (SEM) photograph see Fig. 1,
As seen from Figure 1：Gold nanometer cage is uniform in size and has been stably adhered to carbon ion liquid electrode surface.
（Test case 1）
Gold nanometer cage modified carbon ionic liquid electrode made from test case 1（AuNCs/CILE is referred to as below）And example
1 the step of 2. obtained carbon ion liquid electrode（CILE is referred to as below）Detect the cyclic voltammetric response of cyanidenon.
Test condition is as follows：Cyanidenon concentration 1.0 × 10-6Mol/L, electrolyte solution are phosphate buffer（pH=
3.0）, working electrode is respectively AuNCs/CILE and CILE, and auxiliary electrode is platinized platinum, and reference electrode is saturation calomel electricity
Pole, potential window are 0.7V~0.1V, sweep speed 0.1V/s, as a result see Fig. 2.Wherein, curve a represents AuNCs/CILE,
Curve b represents CILE.
（Test case 2）
Test the cyclic voltammetric response of AuNCs/CILE detections cyanidenon under different scanning speed.
Test condition is as follows：Cyanidenon concentration 1.0 × 10-6Mol/L, electrolyte solution are phosphate buffer（pH=
3.0）, working electrode AuNCs/CILE, auxiliary electrode is platinized platinum, and reference electrode is saturated calomel electrode, and potential window is
0.7V~0.1V, as a result see Fig. 3.Wherein, a to j represent respectively 0.02V/s, 0.04V/s, 0.06V/s, 0.08V/s, 0.1V/s,
0.14V/s, 0.18V/s, 0.22V/s, 0.26V/s, 0.3V/s sweep speed.
As seen from Figure 3：All occur a pair of redox peaks under different scanning speed, and with preferably symmetrical
Property, illustrate that electrode reaction has good invertibity.
（Test case 3）
With differential pulse voltametry（DPV）Test the oxidation peak electricity of the luteolin solution of AuNCs/CILE detection various concentrations
Stream.
Test condition is as follows：Electrolyte solution is phosphate buffer（pH=3.0）, working electrode AuNCs/CILE is auxiliary
It is platinized platinum to help electrode, and reference electrode is saturated calomel electrode, and potential window is 0.35V~0.65V, sweep speed 0.1V/s,
As a result Fig. 4 is seen.Wherein, a to j represents 0.04,0.08,0.6,0.8,1,2,4,6,8,10 μm of ol/L respectively.
As seen from Figure 4：As cyanidenon concentration constantly increases, oxidation peak current is also constantly increasing.
（Test case 4）
Test the cyclic voltammetric response that AuNCs/CILE in the phosphate buffer of different pH value detects cyanidenon.
Test condition is as follows：Cyanidenon concentration 1.0 × 10-6Mol/L, working electrode AuNCs/CILE, auxiliary electrode
For platinized platinum, reference electrode is saturated calomel electrode, and potential window is 0.7V~0.1V, sweep speed 0.1V/s, as a result sees figure
5.Wherein, a to g represents pH value as 2.0,3.0,4.0,5.0,6.0,7.0,8.0 respectively.
As seen from Figure 5：The pH of phosphate buffer during redox peak current maximum be 3.0, that is, select pH for
3.0 phosphate buffer is electrolyte solution.
（Test case 5）
Test the Middle Eocene that AuNCs/CILE in the phosphate buffer of different pH value detects cyanidenon.
Test condition is as follows：Cyanidenon concentration 1.0 × 10-6Mol/L, working electrode AuNCs/CILE, auxiliary electrode
For platinized platinum, reference electrode is saturated calomel electrode, sweep speed 0.1V/s, as a result sees Fig. 6.
As seen from Figure 6：In pH（2.0~7.0）In the range of, Middle Eocene（E0'）Good linear relationship is presented with pH,
And it is E to fit a linear equation0'=-0.0613pH+0.679（γ=0.993）, slope is -61.3mV/pH and theoretical value
It is close.
Illustrate that the oxidation-reduction process that cyanidenon occurs on AuNCs/CILE is to wait the proton processes such as electronics.
（Test case 6）
Ac impedance measurement comparison is carried out to AuNCs/CILE and CILE.
Test condition is as follows：[Fe(CN)]3-/4-（Concentration is 1.0mol/L）And KCl（Concentration is 0.1mol/L）Mixed liquor,
Frequency range is 0.1~105Hz, AC bias 5mV, current potential 0.202V.
The charge transfer resistance of electrode interface is solved by the semicircle of high frequency region（Ret）, as a result see Fig. 7.Wherein, curve a generations
Table CILE, curve b represent AuNCs/CILE.
As seen from Figure 7：AuNCs modifications cause the resistance value at interface to reduce after arriving CILE surfaces, and this is due to AuNCs
With good electric conductivity, big specific surface area provides express passway for electric charge transfer.
（Test case 7）
Influence of the different material to cyanidenon electro-chemical test.
Test condition is as follows：Cyanidenon concentration 1.0 × 10-6Mol/L, electrolyte solution are phosphate buffer（pH=
3.0）, working electrode AuNCs/CILE, auxiliary electrode is platinized platinum, and reference electrode is saturated calomel electrode, and potential window is
0.7V~0.1V, sweep speed 0.1V/s.
Be separately added into 50 times sodium ion, barium ions, potassium ion, cadmium ion, manganese ion, cobalt ions, lysine, Soviet Union ammonia
Acid, glycine and alanine, test the influence to cyanidenon electrochemical behavior, the results are shown in Table 1.
As can be seen from Table 1：Gained relative error is respectively less than 5%, illustrates that this method has preferably selectivity.
（Application examples）
The method that the application example detects content of luteolin in Radix Lamiophlomidis Rotatae capsule for AuNCs/CILE made from example 1.
S1：10 Radix Lamiophlomidis Rotatae capsules are taken, soaked in absolute ethyl alcohol is first used after removing capsule shell, is then heated to reflux 2h, mistake
Filter, filtrate are diluted with the phosphate buffer of pH=3, obtain sample solution；
The Radix Lamiophlomidis Rotatae capsule that the application example uses is purchased from Gansu lamiophlomis rotata pharmaceutical Co. Ltd（Chinese medicines quasi-word Z10970053）.
S2：Using AuNCs/CILE made from example 1 as working electrode, platinized platinum is auxiliary electrode, and saturated calomel electrode is ginseng
Than electrode, the relation of the peak point current and its gradient concentration of cyanidenon is detected by Differential Pulse Voltammetry, establishes standard song
Line；
S3：By cyanidenon standard liquid（1.0×10-6mol/L）It is added in the sample solution of above-mentioned steps S1 preparations, enters
The row rate of recovery is tested, and determines the rate of recovery.
As a result the rate of recovery is shown in the range of 97.8%~99.0%, shows that AuNCs/CILE made from example 1 can be applied to
The measure of content of luteolin in Radix Lamiophlomidis Rotatae capsule.
Claims (8)
1. a kind of method for detecting content of luteolin in Radix Lamiophlomidis Rotatae capsule, has steps of：
S1：Prepare Radix Lamiophlomidis Rotatae capsule sample solution；
S2：Using chemically modified electrode as working electrode, platinized platinum is auxiliary electrode, and saturated calomel electrode is reference electrode, by showing
The relation of the peak point current and its gradient concentration of poor pulse voltammetry detection cyanidenon, establishes standard curve；Described chemistry
Modified electrode is gold nanometer cage modified carbon ionic liquid electrode；
S3：Cyanidenon standard liquid is added in the sample solution of above-mentioned steps S1 preparations, carries out rate of recovery experiment, measure
The rate of recovery.
2. the method for content of luteolin in detection Radix Lamiophlomidis Rotatae capsule according to claim 1, it is characterised in that：Above-mentioned step
The preparation process of Radix Lamiophlomidis Rotatae capsule sample solution is as follows described in rapid S1：It will be soaked after Radix Lamiophlomidis Rotatae capsule removal shell with absolute ethyl alcohol
Steep and flow back, then filter, filtrate produces after being diluted with phosphate buffer, and the wherein pH of phosphate buffer is 3.
3. the method for content of luteolin in detection Radix Lamiophlomidis Rotatae capsule according to claim 1, it is characterised in that：Above-mentioned step
The concentration of cyanidenon standard liquid described in rapid S3 is 1.0 × 10-6mol/L。
4. the method for content of luteolin, its feature exist in the detection Radix Lamiophlomidis Rotatae capsule according to one of claims 1 to 3
In：The preparation method of chemically modified electrode described in above-mentioned steps S2 is as follows：
1. 1- hexyl pyridine hexafluorophosphates and graphite powder are ground uniformly, carbon ion liquid paste is obtained；
2. inserting in vitreous electricity pole pipe and being compacted 1. carbon ion liquid that step obtains paste, be inserted into copper wire, obtain carbon from
Sub- liquid electrode；
3. 2. carbon ion liquid electrode surface that the uniform drop coating of gold nanometer cage to step is obtained, dry in the shade and produce gold nanometer cage modification
Carbon ion liquid electrode.
5. the method for content of luteolin in detection Radix Lamiophlomidis Rotatae capsule according to claim 4, it is characterised in that：Above-mentioned step
Suddenly 1. described in the weight ratio of 1- hexyl pyridine hexafluorophosphates and the graphite powder be 1: 1~1: 3.
6. a kind of preparation method for detecting the chemically modified electrode used in Radix Lamiophlomidis Rotatae capsule in the method for content of luteolin, its
It is characterized by following steps：
1. 1- hexyl pyridine hexafluorophosphates and graphite powder are ground uniformly, carbon ion liquid paste is obtained；
2. inserting in vitreous electricity pole pipe and being compacted 1. carbon ion liquid that step obtains paste, be inserted into copper wire, obtain carbon from
Sub- liquid electrode；
3. 2. carbon ion liquid electrode surface that the uniform drop coating of gold nanometer cage to step is obtained, dry in the shade and produce gold nanometer cage modification
Carbon ion liquid electrode.
7. preparation method according to claim 6, it is characterised in that：Above-mentioned steps 1. described in 1- hexyl pyridine hexafluoro phosphorus
The weight ratio of hydrochlorate and the graphite powder is 1: 1~1: 3.
8. the gold nanometer cage modified carbon ionic liquid electrode that the preparation method described in a kind of claim 6 or 7 obtains.
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Cited By (7)
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|---|---|---|---|---|
| CN108535339A (en) * | 2018-03-28 | 2018-09-14 | 海南师范大学 | Nanogold-biomass carbon composite material modified electrode and its application in cyanidenon detection |
| CN108760847A (en) * | 2018-06-07 | 2018-11-06 | 海南师范大学 | A kind of method that electrostatic spinning prepares zinc oxide-carbon nano-fiber composite material and its modified electrode with high temperature cabonization method |
| CN108914253A (en) * | 2018-05-31 | 2018-11-30 | 海南师范大学 | A method of carbon nano-fiber and its modified electrode are prepared based on electrostatic spinning and high temperature cabonization |
| CN108950735A (en) * | 2018-06-07 | 2018-12-07 | 海南师范大学 | A kind of method of electrostatic spinning prepares the preparation of carbon nano-fiber-hydroxyapatite composite material method and its modified electrode |
| CN109164150A (en) * | 2018-10-09 | 2019-01-08 | 海南师范大学 | A kind of preparation of gold nanometer cage modified electrode and the method for detecting rutin content |
| CN110161096A (en) * | 2019-04-30 | 2019-08-23 | 海南师范大学 | A kind of application of preparation based on platinum-biomass carbon nanocomposite electrochemical sensor and luteolin detection |
| CN110361435A (en) * | 2019-08-09 | 2019-10-22 | 嘉兴学院 | A kind of glass-carbon electrode and preparation method and application of ion liquid modified montmorillonite modification |
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| CN108535339A (en) * | 2018-03-28 | 2018-09-14 | 海南师范大学 | Nanogold-biomass carbon composite material modified electrode and its application in cyanidenon detection |
| CN108914253A (en) * | 2018-05-31 | 2018-11-30 | 海南师范大学 | A method of carbon nano-fiber and its modified electrode are prepared based on electrostatic spinning and high temperature cabonization |
| CN108914253B (en) * | 2018-05-31 | 2023-09-29 | 海南师范大学 | Method for preparing carbon nanofiber and modifying electrode thereof based on electrostatic spinning and high-temperature carbonization |
| CN108760847A (en) * | 2018-06-07 | 2018-11-06 | 海南师范大学 | A kind of method that electrostatic spinning prepares zinc oxide-carbon nano-fiber composite material and its modified electrode with high temperature cabonization method |
| CN108950735A (en) * | 2018-06-07 | 2018-12-07 | 海南师范大学 | A kind of method of electrostatic spinning prepares the preparation of carbon nano-fiber-hydroxyapatite composite material method and its modified electrode |
| CN109164150A (en) * | 2018-10-09 | 2019-01-08 | 海南师范大学 | A kind of preparation of gold nanometer cage modified electrode and the method for detecting rutin content |
| CN110161096A (en) * | 2019-04-30 | 2019-08-23 | 海南师范大学 | A kind of application of preparation based on platinum-biomass carbon nanocomposite electrochemical sensor and luteolin detection |
| CN110361435A (en) * | 2019-08-09 | 2019-10-22 | 嘉兴学院 | A kind of glass-carbon electrode and preparation method and application of ion liquid modified montmorillonite modification |
| CN110361435B (en) * | 2019-08-09 | 2021-11-09 | 嘉兴学院 | Ionic liquid modified montmorillonite modified glassy carbon electrode and preparation method and application thereof |
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