CN109541006A - It is a kind of for measuring the novel electrode and its measuring method of Metformin hydrochloride - Google Patents
It is a kind of for measuring the novel electrode and its measuring method of Metformin hydrochloride Download PDFInfo
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Abstract
The present invention relates to a kind of preparation of novel electrode for Metformin Hydrochloride Detection and its electrochemical methods.The measurement system is working electrode by N-N dimethylformamide/nano silver modified conducting glass electrode, and saturated calomel electrode is reference electrode, and platinum electrode is to form to electrode.This method be 6.64 using pH PBS as buffer solution, within the scope of 0 ~ 1V of current potential, under conditions of scanning speed 50mV/s, measure the oxidation peak current of cyclic voltammetry curve.Determination of metformin hydrochloride linear relationship within the scope of 0.075 ~ 0.2mg/mL is good.Its calibration curve equation is y=31.719x+3.0076, R2=0.9595.10 times the average recovery rate for measuring Metformin hydrochloride content in same sample lots is 103.5%, and relative standard deviation RSD value is 4.2%.Show that the electrode can be applied to the measurement of active constituent content in Metformin hydrochloride drug sample.
Description
Technical field
The present invention relates to electrochemical analysis detection technique fields, and in particular to the Novel electric for Metformin Hydrochloride Detection
The preparation method and detection method of pole and the electrode.
Background technique
Metformin hydrochloride is a kind of drug for being usually used in reducing blood glucose, is mainly used for occurring hyperglycemia to empty stomach and after the meal
Patients with NIDDM, especially have certain curative effect to fatter and patient that is having hyperinsulinemia, not only can be with
For reducing blood glucose, fat and alleviation hyperinsulinemia can also be reduced.At present people to the detection of Metformin hydrochloride
A large amount of research has been done, the detection method of many Metformin hydrochlorides has also been developed, mainly there is RP HLPC
Method, HPLC method, electrocapillary phoresis method, ultraviolet spectrophotometry and electrochemical process.Since electrochemical process detects Metformin hydrochloride
Compared to other methods stability, sensitivity all has greatly improved, so it has received in Metformin hydrochloride detection field
Greatly pay attention to, has also obtained very big development.
Summary of the invention
The purpose of the present invention is to provide a kind of pair of Metformin hydrochloride selectivity with higher, higher sensitivity,
And it is easier the electrochemical methods of operation.
To achieve the above object, the technical solution adopted by the present invention are as follows: provide a kind of for Metformin Hydrochloride Detection
Novel electrode, including N-N dimethylformamide/nano silver modified conducting glass electrode is working electrode, platinum electrode be to electrode,
Saturated calomel electrode is the three-electrode system of reference electrode composition.
Further, the N-N dimethylformamide/nano silver electrode the preparation method comprises the following steps: platinum electrode be to electrode,
Saturated calomel electrode is that the three-electrode system of reference electrode composition is placed in N-N dimethylformamide；In 0~1V potential range
Between 100mV/s sweep fast scan round 5 weeks, until cyclic voltammetry curve is stablized；Electrode is taken out, by the electrode then in 5mmol/
In the silver nitrate solution of L, in static condition, between -0.2~-0.8V potential range, it is 0.5mV/s that speed is swept in linear dissolution,
Dissolution time is 180s, finally obtains N-N dimethylformamide/nano silver electrode.
Utilize a kind of method of novel electrode measurement Metformin hydrochloride for Metformin Hydrochloride Detection, packet
Include following steps: by N-N dimethylformamide/nano silver modified conducting glass electrode system be placed in concentration be 0.075~
In the standard solution of the Metformin hydrochloride of 0.2mg/mL, the PBS for being 6.64 using pH is buffer solution, in 0~1V of potential range,
Under conditions of scanning speed 50mV/s, the oxidation peak current of cyclic voltammetry curve is recorded, it is then dense to standard items with the current value
Degree is standard curve, standard curve y=31.719x+3.0076, R2=0.9595, under same experimental conditions, measure sample
The peak current of product calculates sample size with the calibration curve equation.
The present invention has good electric conductivity using conductive glass electrode, and combines N-N dimethylformamide, silver nitrate
Property, a kind of pair of Metformin hydrochloride, which is made, has highly sensitive electrode.Then pass through optimization N-N dimethylformamide scanning
Circle number, the type of buffer solution, scanning speed, the parameters such as bottom liquid pH value are obtained to the choosing with higher of N-N dimethylformamide
Selecting property, higher sensitivity, and it is easier operation electrochemical analysis method, and this method is applied to actual sample measurement.
Detailed description of the invention
Below in conjunction with attached drawing, the present invention is further illustrated.
Attached drawing 1 is cyclic voltammogram of the Different electrodes in potassium ferricyanide solution.
Working electrode corresponding to the order of oxidation peak current value from high to low is respectively 1~5 in cyclic voltammetry curve.It is bent
Line 1 is N-N dimethylformamide/nano silver modified conducting glass electrode；Curve 2 is N-N dimethylformamide modified conducting glass
Glass electrode；Curve 3 is nano silver modified conducting glass electrode；Curve 4 is nano silver/N-N dimethylformamide modified conducting glass
Glass electrode；Curve 5 is naked conductive glass electrode.
Attached drawing 2 is cyclic voltammetry curve of the Different electrodes in the Metformin hydrochloride solution of 0.1mg/mL.
(a) nano silver modified conducting glass electrode；(b) N-N dimethylformamide/nano silver modified conducting glass electrode；
(c) nano silver/N-N dimethylformamide modified conducting glass electrode；(d) N-N dimethylformamide modified conducting glass electrode；
(e) naked conductive glass electrode.
Attached drawing 3 is scanning figure of the Metformin hydrochloride of various concentration in modification nano silver electrode.
Attached drawing 4 is the Optimal Curve of pH.
Attached drawing 5 is polymeric membrane (N-N dimethylformamide) thickness optimization curve.
Attached drawing 6 is that the CV of various concentration Metformin hydrochloride solution schemes.
Attached drawing 7 is double with hydrochloride of the N-N dimethylformamide/nano silver modified conducting glass electrode to various concentration
The oxidation peak of guanidine solution I-V Characteristic Analysis figure, the standard curve made.
Specific embodiment
Implementing though of the invention are as follows:
The preparation of sensor: the purification of glass electrode (ITO), cyclic voltammetry scan N-N dimethylformamide, electro-deposition
Prepare N-N dimethylformamide/nano silver modified electrode；
The optimization of determination condition: the influence of the circle number of nitrogen is modified in the type of buffer solution, the influence of pH, scanning speed
It influences；
The measurement of actual sample: working electrode be with N-N dimethylformamide that electro-conductive glass (ITO) is base electrode/
Nano silver modified electrode, reference electrode are saturated calomel electrode (SCE), are platinum electrode to electrode, are assembled into three-electrode system；
The three-electrode system is placed in the PBS (2 × 10 for being 6.64 with pH-6G/ml catechol) buffer solution configuration hydrochloride it is double
In guanidine solution, recording peak current in concentration with optimum experimental condition is the cyclic voltammetry curve within the scope of 0.05~0.2mg/ml.
It is specific:
The purification of glass electrode: electro-conductive glass (ITO) is successively used into detergent, dilute hydrochloric acid, ethyl alcohol, deionized water ultrasound is clearly
Wash 5min, cold wind drying.
Preparation N-N dimethylformamide/nano silver modified electrode: whole preparation process is all to utilize CS300 electrochemistry work
Make station to carry out, use three-electrode system: electro-conductive glass (ITO) is working electrode for base electrode, and platinum electrode is to satisfy to electrode
It is reference electrode with calomel electrode (SCE).Assembled three-electrode system is put into N-N dimethylformamide static first
Under conditions of, 100mV/s sweeps fast scan round 5 weeks between 0~1V potential range, until cyclic voltammetry curve is stablized, takes out
Electrode, by the electrode then in the silver nitrate solution of 5mmol/L, in static condition, in -0.2~-0.8V potential range it
Between, it is 0.5mV/s, dissolution time 180s that speed is swept in linear dissolution.N-N dimethylformamide/nano silver electrode is made.
As shown in Fig. 1, cyclic voltammogram of the Different electrodes in potassium ferricyanide solution.Successively use 1.N-N dimethyl methyl
Amide/nano silver electrode；2.N-N dimethylformamide electrode；3. nano silver electrode；4. nano silver/N-N dimethylformamide electricity
Pole；5. naked glass electrode is 1.5 × 10-2mol/L K3[Fe(CN)6] (current level 0 is scanned using cyclic voltammetry in solution
~1V, scanning speed 50mV/s).N-N dimethylformamide electrode (curve 2) in figure, nano silver electrode (curve 3) nano silver/
N-N dimethylformamide electrode (curve 4) more naked glass electrode (curve 5) redox peak current increases, and shows N-N dimethyl
Formamide, nano silver, nano silver/N-N dimethyl formyl have all been aggregated to glass electrode surface respectively, have promoted probe ion and exist
The redox of electrode surface.And the N-N dimethylformamide obtained when N-N dimethylformamide surface modification silver nitrate/
Nano silver electrode (curve 1) oxidation current peak highest, but as can be seen from the figure N-N dimethylformamide/nano silver electrode is (bent
Line 1) reduction peak it is low compared with other electrodes (more naked glass electrode curve 5 is high), illustrate nanometer modified by silver to N-N dimethylformamide
Electric conductivity (oxidation current) is best on electrode.
As shown in Fig. 2, cyclic voltammetry curve of the Different electrodes in the Metformin hydrochloride solution of 0.1mg/mL.Use pH
The concentration of=6.64 (catechol) buffer preparations is the Metformin hydrochloride solution of 0.1mg/mL, successively with repairing nano silver
Electrode, N-N dimethylformamide/nano silver electrode, N-N dimethylformamide electrode, naked conductive glass electrode, nano silver/N-N
Dimethylformamide electrode between 0~1V potential range under 50mV/s scanning speed, the cyclic voltammetric of Different electrodes scanning
Scanning, as can be seen from the figure (b) N-N dimethylformamide/nano silver electrode peak type is best, (d) N-N dimethylformamide electricity
Pole and (e) naked conductive glass electrode not appearance in scanning sample, (c) nano silver/N-N dimethylformamide electrode is in the sample
In oxidation peak be lower than N-N dimethylformamide/nano silver electrode oxidation peak, (a) nano silver electrode oxidation peak be higher than (b).
As shown in Fig. 3, scanning curve of the Metformin hydrochloride of various concentration in modification nano silver electrode.With nanometer
For silver electrode to the 0.075mg/mL prepared with above-mentioned condition, 0.1mg/mL, 0.15mg/mL, 0.2mg/mL Metformin hydrochloride is molten
The linear graph (obtaining linear graph from oxidation peak current value) of liquid cyclic voltammetry scan.As can be seen from the figure oxidation peak linear equation
For y=-129.98x+86.016, R2=0.4108 it can be concluded that silver electrode it is linear bad.
To sum up, know N-N dimethylformamide/nano silver electrode to Metformin hydrochloride by attached drawing 1, attached drawing 2, attached drawing 3
Response it is best.
As shown in Fig. 4, the optimal conditions of pH.With N-N dimethylformamide/nano silver electrode to by pH range be 5~9
PBS (containing catechol) buffer preparation 0.1mg/mL Metformin hydrochloride solution carry out cyclic voltammetry scanning
The curve arrived.As can be seen from the figure with the raising of pH value of buffer solution, oxidation peak current is increasing, when pH is greater than 6.64
Oxidation peak current is reducing.It can thus be appreciated that N-N dimethylformamide/nano silver electrode is to hydrochloric acid in buffer solution pH=6.64
The response of melbine is best.Therefore the invention uses PBS (containing catechol) buffer solution of pH=6.64 as the bottom of as
The measurement of liquid progress Metformin hydrochloride.
As shown in Fig. 5, polymeric membrane (N-N dimethylformamide) thickness optimization curve.With only change N-N dimethyl formyl
Cyclic voltammetry scan circle number in amine, circle number range are that 1~15 circle obtains (different film thicknesses) N-N dimethylformamide/nano silver
Electrode carries out the curve that cyclic voltammetry scan obtains in the Metformin hydrochloride solution of 0.1mg/mL respectively.It can from figure
Out as the increase oxidation peak current of scanning circle number is increasing, reducing when circle number is greater than 5 oxidation peak currents.It can thus be appreciated that sweeping
N-N dimethylformamide/the nano silver electrode retouched when circle number is 5 is best to the response of Metformin hydrochloride.So this experiment with
5 circle numeral system of scanning is for electrode.
As shown in Fig. 6, the CV figure of various concentration Metformin hydrochloride solution.Take the time current figure of oxidation peak.Use pH
It is (bent for 0.05mg/mL (curve 5), 0.075mg/mL that=6.64 PBS (catechol) buffer solution prepares solution concentration respectively
Line 4), the Metformin hydrochloride solution of 0.1mg/mL (curve 3), 0.15mg/mL (curve 2), 0.2mg/mL (curve 1), most
Under good experiment condition, modified electrode measurement is carried out with Metformin hydrochloride solution of the cyclic voltammetry to various concentration.From figure
It can be seen that peak current successively increases and peak type is fine, can be from pattern as Metformin hydrochloride solution concentration increases
Judge that N-N dimethylformamide/nano silver electrode is very high to Metformin hydrochloride drug monitoring sensitivity.
Attached drawing 7 is standard curve.With N-N dimethylformamide/nano silver electrode to the Metformin hydrochloride of various concentration
The oxidation peak of solution I-V Characteristic Analysis figure makes canonical plotting using graphics software.As can be seen from the figure with hydrochloric acid
Determination of metformin increases peak current and is also increasing, it is known that Determination of metformin hydrochloride presents with peak current size and is positively correlated
Gesture, and the solution standard curve of modified electrode scanning various concentration Metformin hydrochloride is y=31.719x+ as we know from the figure
3.0076 R2=0.9595 (Y is electric current, unit 10-5A；X is Determination of metformin hydrochloride, unit mg/mL).
By attached drawing 6, attached drawing 7 may determine that N-N dimethylformamide/nano silver electrode to the essence of Metformin Hydrochloride Detection
Degree and stability are fine.
Under the optimal experiment condition obtained according to above-mentioned experiment, under same experimental conditions, the mark of preparation is measured
The mark concentration for being worth the Metformin hydrochloride drug of (500mg/ piece) is the oxidation peak current 6.2112 of 0.1mg/mL (100mg/L)
×10-5A, calculating sample concentration with the calibration curve equation is 0.1010mg/mL, and every content of drug is 505mg.10 measurements
The average recovery rate of Metformin hydrochloride content is 103.5% in same sample lots, and relative standard deviation RSD value is 4.2%.
The present invention has good electric conductivity using conductive glass electrode, and combines N-N dimethylformamide, silver nitrate
Property, a kind of pair of Metformin hydrochloride, which is made, has highly sensitive electrode.Then pass through optimization N-N dimethylformamide scanning
Circle number, the type of buffer solution, scanning speed, the parameters such as bottom liquid pH value are obtained to the choosing with higher of N-N dimethylformamide
Selecting property, higher sensitivity, and it is easier operation electrochemical analysis method, and this method is applied to actual sample measurement.
Claims (3)
1. a kind of for measuring the novel electrode of Metformin hydrochloride, which is characterized in that the novel electrode is N-N dimethyl methyl
Amide/nano silver modified conducting glass electrode, wherein N-N dimethylformamide/nano silver modified conducting glass electrode is work
Electrode, platinum electrode are to electrode, saturated calomel electrode be reference electrode composition three-electrode system.
2. preparing a kind of method for measuring the novel electrode of Metformin hydrochloride as described in claim 1, feature exists
In the preparation method includes:
It will take electro-conductive glass as base electrode as working electrode, platinum electrode is to electrode, and saturated calomel electrode is reference electrode
The three-electrode system of composition is placed in N-N dimethylformamide；100mV/s's sweeps fast circulation between 0~1V potential range
Scanning 5 weeks, until cyclic voltammetry curve is stablized；Electrode is taken out, by the electrode then in the silver nitrate solution of 5mmol/L, quiet
Condition only, between -0.2~-0.8V potential range, linear dissolution sweeps speed for 0.5mV/s, dissolution time 180s, finally
Obtain N-N dimethylformamide/nano silver modified conducting glass electrode.
3. a kind of method using a kind of novel electrode measurement borax for borax measurement described in claim 1, feature
It is, which includes:
N-N dimethylformamide/nano silver electrode system is placed in the Metformin hydrochloride that concentration is 0.075~0.2mg/mL
In standard solution, the PBS for being 6.64 using PH is buffer solution, under conditions of 0~1V of potential range, scanning speed 50mV/s,
The oxidation peak current for recording cyclic voltammetry curve, then does standard curve, standard curve to standard concentration with the current value
For y=31.719x+3.0076, R2=0.9595, wherein y is electric current, current unit 10-5A, x are Determination of metformin hydrochloride,
Unit is mg/mL, under same experimental conditions, measures the peak current of sample, calculates sample size with the calibration curve equation.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114994153A (en) * | 2022-06-07 | 2022-09-02 | 青岛理工大学 | Preparation method and application of electrochemical sensor for rapidly detecting metformin |
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| CN103852499A (en) * | 2012-11-29 | 2014-06-11 | 北京市药品检验所 | Method used for rapid detection of illegally added biguanide compound in product |
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Cited By (2)
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| CN114994153A (en) * | 2022-06-07 | 2022-09-02 | 青岛理工大学 | Preparation method and application of electrochemical sensor for rapidly detecting metformin |
| CN114994153B (en) * | 2022-06-07 | 2023-07-25 | 青岛理工大学 | Preparation method and application of electrochemical sensor for rapidly detecting metformin |
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