CN100465622C - Method for capillary electrophoresis electrochemiluminescence detection of metoprolol and atenolol - Google Patents

Method for capillary electrophoresis electrochemiluminescence detection of metoprolol and atenolol Download PDF

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CN100465622C
CN100465622C CNB2006101733908A CN200610173390A CN100465622C CN 100465622 C CN100465622 C CN 100465622C CN B2006101733908 A CNB2006101733908 A CN B2006101733908A CN 200610173390 A CN200610173390 A CN 200610173390A CN 100465622 C CN100465622 C CN 100465622C
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atenolol
metoprolol
solution
concentration
hpo
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CN1995983A (en
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由天艳
黄建设
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Changzhou Institute Of Energy Storage Materials & Devices
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Changchun Institute of Applied Chemistry of CAS
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Abstract

The invention relates to electrocapillarity electrophoresis electrochemiluminescence inspection. It makes direct analysis for the standard sample solution and marked urine sample. It has high sensitivity and simple operation. The inspection linear scope for two standard solutions are 5*10-8-1. 0*10-5mol/L and 7. 5*10-8-1. 0*10-6mol/L, lower limit 5. 0*10-9mol/L and 7. 5*10-8mol/L. It can also be used for betaantagonist analysis with far reaching significance in betaantagonist clinical inspection.

Description

The method of capillary electrophoresis electrochemiluminescdetection detection of metoprolol and atenolol
Technical field
The invention belongs to capillary electrophoresis electrochemical light-emitting detection technique field, be specifically related to the method for capillary electrophoresis electrochemiluminescdetection detection of metoprolol and atenolol.
Background technology
Metoprolol and atenolol belong to β (1)-adrenoreceptor inhibitor class medicine, are widely used in the treatment of angiocardiopathies such as hypertension, angina pectoris, arrhythmia cordis and miocardial infarction.Because it has sedation, also is used as excitant in sports.Such medicine of excessive use can cause that heartbeat is releived, low blood pressure, bronchial spasm and hypoglycemia etc.So the analytical approach of such medicine of detection of development rapid sensitive has great importance at aspects such as clinical examination, Doping Controls and pharmacokinetics.
At present the detection of this type of medicine is mainly used the method for chromatograph-mass spectrometer coupling, comprised UV-VIS spectrophotometry, differentiated pulse voltammetry or the like in addition.The chromatograph-mass spectrometer coupling technology can also provide the structural information of analyte simultaneously except highly sensitive, be a kind of important method of Pharmaceutical Analysis detection range.But the instrument and equipment that chromatography-mass spectroscopy needs structure is meticulous, and the instrument expense is higher.Capillary Electrophoresis has reagent and the sample consumption is little, efficiently, advantage such as separating power fast, is applicable to the separation of various ions and neutral substance, is compartment analysis means with fastest developing speed in recent years.Ru (bpy) 3 2+It is a kind of highly sensitive detection method that electrochemiluminescence detects, and has been widely used in the analyzing and testing of amino acid, protein, DNA and organic amine material.It is low, simple to operate that capillary electrophoresis electrochemical light-emitting detects the required instrument cost of coupling technique, and the compartment analysis ability is strong.
Summary of the invention
The method that the purpose of this invention is to provide capillary electrophoresis electrochemiluminescdetection detection of metoprolol and atenolol.Be specifically related to the method for a kind of capillary electrophoresis electrochemical light-emitting analyzing and testing metoprolol and atenolol.
The used apparatus of this method is: internal diameter 25 μ m not coating melt silicon capillary; Diameter 500 μ mPt coil working electrode, the saturated KCl solution of Ag/AgCl/ contrast electrode, Pt silk auxiliary electrode; MPI-A type capillary electrophoresis electrochemical light-emitting detector.
Agents useful for same is: Ru (bpy) 3Cl 26H 2O, NaH 2PO 4, Na 2HPO 4, H 3PO 4, NaOH, metoprolol and atenolol standard items; It is pure that agents useful for same is analysis; All solution are all with secondary water preparation, the solution for preparing before using all through 0.22 μ m membrane filtration.
Analyzing and testing to metoprolol and atenolol is divided into following step:
1), for the sensitivity that guarantees to detect and the reappearance of analysis result, need do following processing to kapillary and working electrode
(1), kapillary before using for the first time, wash with 0.1mol/L NaOH solution and to spend the night; In operating process, spend the night with the flushing of 0.1mol/L NaOH solution every day, more respectively with secondary power and water swimming damping fluid flushing capillary column 2-10min, balance 2-10min under separation condition at last;
(2), diameter 500 μ mPt dish working electrode before operation at 1.0mol/L H 2SO 4In the solution, in-0.2-1.5V potential range, circulate and sweep, up to the feature cyclic voltammetry curve that obtains the Pt electrode.With working electrode scan round 10-20 week in detection cell buffer solution, the scanning potential range is 0-1.35V in the operating process, to remove the electrode surface pollutant, the activation working electrode;
2), the preparation of buffer solution
(1), the compound method of the buffer solution of pH＜5.0 is:
Elder generation's compound concentration is the NaH of 10-50mmol/L 2PO 4Solution and concentration are the H of 1.0mol/L 3PO 4Solution is used the H of 1.0mol/L then 3PO 4Solution is adjusted to pH＜5.0;
(2), the compound method of the buffer solution of 5.0≤pH≤9.0 is:
Compound concentration is the NaH of 10-100mmol/L respectively earlier 2PO 4And Na 2HPO 4Solution will can obtain the buffer solution of 5.0≤pH≤9.0 with the two mixing of concentration;
(3), pH〉compound method of 9.0 buffer solution is:
Elder generation's compound concentration is the Na of 10-100mmol/L 2HPO 4Solution and concentration are the NaOH solution of 1.0mol/L, and the NaOH solution with 1.0mol/L is adjusted to pH then〉9.0;
3), the preparation of metoprolol and atenolol standard solution and static experiment thereof
The concentration of metoprolol and atenolol storing solution is 1.0mmol/L, and storing solution keeps in Dark Place in 4 ℃ of refrigerators;
The static state experiment of metoprolol and atenolol standard solution:
With 100mmol/L, the NaH of pH 7.5 2PO 4-Na 2HPO 4Buffer solution is electrolyte as a setting, and sweep interval is 0-1.35V, cyclic voltammetric (CV) curve and electrochemiluminescence (ECL) curve when record is stablized; Scan round in the back-ground electolyte that contains 0.4mmol/L metoprolol and atenolol then, sweep interval is similarly 0-1.35V, CV curve and ECL curve when record is stablized; With the contrast of CV curve and the ECL curve and the back-ground electolyte of metoprolol and atenolol, whether has enhancing Ru (bpy) to determine metoprolol and atenolol 3 2+The electrochemiluminescence activity.
4), CE-ECL detects the testing conditions of metoprolol and atenolol standard solution, and carries out the investigation of the range of linearity and detectability with this understanding
Select the constant potential mode of operation, change-detection current potential between 1.0-1.3V; 2-10s changes sample injection time and sample introduction high pressure between the 10-15kV; Change between the 10-20kV and separate high pressure; 10.0-50.0mmol/L between change NaH 2PO 4-Na 2HPO 4The electrophoresis buffer concentration changes NaH between the 5.0-9.0 2PO 4-Na 2HPO 4The electrophoresis pH value of buffer solution; NaH in the detection cell 2PO 4-Na 2HPO 4Electrophoresis buffer solution is fixed as 100mmol/L, and the pH value changes between 5.0-9.0; Ru in the detection cell (bpy) 3 2+Concentration in the 1.0-10.0mmol/L scope, change; The photomultiplier high pressure is 600-900V.
Aspects such as overall sensitivity, peak shape, reappearance determine that the testing conditions of symmetrical no obvious peak broadening of highly sensitive, peak shape and favorable reproducibility is a top condition, and optimal detection condition is: detect current potential 1.15V; Sample injection time 8s, sample introduction high pressure 10kV; Separate high pressure 15kV; NaH 2PO 4-Na 2HPO 4Electrophoresis buffer concentration 10.0mmol/L (pH8.5); 5mMRu (bpy) 3 2+With 100mM NaH 2PO 4-Na 2HPO 4(pH 8.5) join in the detection cell; The photomultiplier high pressure is 800V.
Under optimal detection condition, the detectability of metoprolol and atenolol standard items is respectively 5.0 * 10 -9Mol/L and 7.5 * 10 -8Mol/L, the range of linearity is respectively 5 * 10 -8-1.0 * 10 -5Mol/L and 7.5 * 10 -8-1.0 * 10 -6Mol/L.
5), the investigation of metoprolol and atenolol standard solution separation condition
Sample injection time changes between 1-10s, changes NaH between the 10.0-50.0mmol/L 2PO 4-Na 2HPO 4The electrophoresis buffer concentration changes NaH between the 2.0-5.0 2PO 4-Na 2HPO 4The electrophoresis pH value of buffer solution.
Condition when reaching baseline separation with metoprolol and atenolol is the optimal separation condition, and the optimal separation condition is: 10kV electrokinetic injection 2s; 10.0mmol/LNaH 2PO 4-Na 2HPO 4Electrophoresis buffer solution, pH 3.0.
6), blank urine sample and contain metoprolol and the preparation process of the mark-on urine sample of atenolol standard items
Get healthy people's urine, through 0.22 μ m membrane filtration, afterwards doubly with secondary water dilution 10-20, as blank urine sample; Isopyknic metoprolol and atenolol storing solution added to be made in the blank urine sample contain metoprolol and atenolol standard items concentration is 1.0 * 10 -7-1.0 * 10 -5The mark-on urine sample of mol/L;
7), blank urine sample and contain metoprolol and the detection of the mark-on urine sample of atenolol standard items
5) under the optimal separation testing conditions of gained, obtain blank urine sample and contain metoprolol and the electrophoresis pattern of the mark-on urine sample of atenolol standard items.
The metoprolol involved in the present invention and the detection method of atenolol relatively have following characteristics with other analytical approachs:
1. cost is low, and is simple to operate.Capillary electrophoresis electrochemical light-emitting detects only needs a capillary, a high-voltage power supply, and a potentiostat, a luminous detection instrument and some laboratory common chemical reagent can be finished analysis task; The homogeneity spectrum detection method is compared, and operates simplyr, and instrument cost is also lower.
2. highly sensitive, the range of linearity is wide.This method is respectively 5.0 * 10 to the detection lower limit of metoprolol and atenolol -9Mol/L and 7.5 * 10 -8Mol/L is than low 2 orders of magnitude of the most frequently used ultraviolet detection method detectability, suitable with the testing result of liquid phase chromatogram-mass spectrometry combination method.The range of linearity is respectively 5 * 10 -8-1.0 * 10 -5Mol/L and 7.5 * 10 -8-1.0 * 10 -6Mol/L.
The present invention is applied to the capillary electrophoresis electrochemical light-emitting detection technique detection of metoprolol and atenolol first.Adopting traditional three-electrode system, is working electrode with the Pt disc electrode, and platinum filament is to the utmost point, and Ag/AgCl is a contrast electrode, and buffer solution uses NaH 2PO 4-Na 2HPO 4Damping fluid.
Description of drawings
Fig. 1 is metoprolol and the electrophoresis pattern of atenolol standard items under optimal detection condition.Wherein A is atenolol (AT), and B is metoprolol (ME), and the concentration of AT and ME is 5.0 * 10 -6Mol/L.
Fig. 2 is metoprolol and the electrophoresis pattern of atenolol standard items under the optimal separation condition, and AT and ME concentration are 2.5 * 10 in the standard solution -6Mol/L.
Fig. 3 is the electrophoresis spectrogram that metoprolol and atenolol standard solution add the target urine sample.Wherein A is blank urine sample, and B is that metoprolol and atenolol standard solution add the target urine sample, and the concentration of AT and ME is 2.5 * 10 in the mark-on urine sample -6Mol/L.
Embodiment
Following examples capillary electrophoresis electrochemical light-emitting detector.Working electrode is diameter 500 μ m Pt disc electrodes, and auxiliary electrode is a platinum electrode, and contrast electrode is Ag/AgCl (saturated KCl solution) electrode.Capillary column internal diameter 25 μ m, capillary column endpiece alignment work electrode surface adopts the styletable detecting pattern.
The detection of embodiment 1 metoprolol and atenolol standard items
To the detection of metoprolol and atenolol standard items, used instrument as previously mentioned, it is as follows to detect step:
1. the preparation of metoprolol and atenolol standard solution
Metoprolol and atenolol storing solution concentration are 1.0mmol/L.Storing solution keeps in Dark Place in 4 ℃ of refrigerators.
2.10.0mmol/L, the NaH of pH 8.5 2PO 4-Na 2HPO 4The preparation of buffer solution
Elder generation's compound concentration is the NaH of 10.0mmol/L 2PO 4Solution and concentration are the Na of 10.0mmol/L 2HPO 4Solution mixes both then, and is adjusted to pH 8.5.
3.100.0mmol/L, the NaH of pH 8.5 2PO 4-Na 2HPO 4The preparation of buffer solution
Elder generation's compound concentration is the NaH of 100.0mmol/L 2PO 4Solution and concentration are the Na of 100.0mmol/L 2HPO 4Solution mixes both then, regulates pH value to 8.5.
4. the detection of metoprolol and atenolol standard items
Detecting current potential 1.15V; Electrophoresis buffer concentration 10.0mmol/L, pH 8.5; Sample injection time 8s, sample introduction voltage 10kV; Separate high pressure 15kV; 5mM Ru (bpy) 3 2+And 100mMNaH 2PO 4-Na 2HPO 4(pH 8.5) join in the detection cell; The photomultiplier high pressure is 800V.Under this top condition, metoprolol and atenolol can obtain respectively detecting in the 7min, and under optimal detection condition, the detectability of metoprolol and atenolol standard items is respectively 5.0 * 10 simultaneously -9Mol/L and 7.5 * 10 -8Mol/L, the range of linearity is respectively 5 * 10 -8-1.0 * 10 -5Mol/L and 7.5 * 10 -8-1.0 * 10 -6Mol/L.The electrophoresis pattern of metoprolol and atenolol standard items as shown in Figure 1.
In experimentation,, need kapillary and working electrode are carried out suitable processing for guaranteeing to obtain higher signal response and quite good detecting reappearance.
Disposal route capillaceous is: kapillary spends the night with the flushing of 0.1mol/L NaOH solution before using for the first time.In experimentation, spend the night with the flushing of 0.1mol/L NaOH solution every day, more respectively with secondary power and water swimming damping fluid flushing capillary column 5min, and then static hairlet capillary column 10min under the separation condition.
The disposal route of working electrode is: 500 μ mPt dish working electrode is before use at 1.0mol/LH 2SO 4In the solution, in-0.2-1.5V potential range, circulate and sweep, up to the feature cyclic voltammetry curve that obtains the Pt electrode.With working electrode scan round 10-20 week in detection cell buffer solution, sweep interval is 0-1.35V in the experimentation, to remove the electrode surface pollutant, the activation working electrode surface.
Separation detection in the time of embodiment 2 metoprolols and atenolol standard items
Separation detection in the time of to metoprolol and atenolol standard items, used instrument as previously mentioned, the separation detection step is as follows:
1. the preparation of metoprolol and atenolol standard solution
Metoprolol and atenolol storing solution concentration are 1.0mmol/L.Storing solution keeps in Dark Place in 4 ℃ of refrigerators.
2.10.0mmol/L, the NaH of pH 3.0 2PO 4-Na 2HPO 4The preparation of buffer solution
Elder generation's compound concentration is the NaH of 10.0mmol/L 2PO 4Solution and concentration are the H of 1.0mmol/L 3PO 4Solution is used H then 3PO 4Solution is adjusted to pH 3.0.
3.100.0mmol/L, the NaH of pH 8.5 2PO 4-Na 2HPO 4The preparation of buffer solution
Elder generation's compound concentration is the NaH of 100.0mmol/L 2PO 4Solution and concentration are the Na of 100.0mmol/L 2HPO 4Solution mixes both then, regulates pH value to 8.5.
4. separation detection metoprolol and atenolol standard items the time
Detecting current potential 1.15V; Electrophoresis buffer concentration 10.0mmol/L, pH 3.0; Sample injection time 2s, sample introduction voltage 10kV; Separate high pressure 15kV, 5mM Ru (bpy) 3 2+And 100mMNaH 2PO 4-Na 2HPO 4(pH 8.5) join in the detection cell; The photomultiplier high pressure is 800V.Under this top condition, 20min can obtain separation detection (Fig. 2) simultaneously with interior metoprolol and atenolol.
In experimentation,, need kapillary and working electrode are carried out suitable processing for guaranteeing to obtain higher signal response and quite good detecting reappearance.
Disposal route capillaceous is: kapillary spends the night with the flushing of 0.1mol/L NaOH solution before using for the first time.In experimentation, spend the night with the flushing of 0.1mol/L NaOH solution every day, more respectively with secondary power and water swimming damping fluid flushing capillary column 5min, and then static hairlet capillary column 10min under the separation condition.
The disposal route of working electrode is: 500 μ mPt dish working electrode is before use at 1.0mol/LH 2SO 4In the solution, in-0.2-1.5V potential range, circulate and sweep, up to the feature cyclic voltammetry curve that obtains the Pt electrode.With working electrode scan round 10-20 week in detection cell buffer solution, sweep interval is 0-1.35V in the experimentation, to remove the electrode surface pollutant, the activation working electrode surface.
The separation detection of metoprolol and atenolol in embodiment 3 urine samples
To the separation detection of metoprolol in the urine sample and atenolol, used instrument as previously mentioned, the separation detection step is as follows:
1.10.0mmol/L, the NaH of pH 3.0 2PO 4-Na 2HPO 4The preparation of buffer solution
Elder generation's compound concentration is the NaH of 10.0mmol/L 2PO 4Solution and concentration are the H of 1.0mmol/L 3PO 4Solution is used H then 3PO 4Solution is adjusted to pH 3.0.
2.100.0mmol/L, the NaH of pH 8.5 2PO 4-Na 2HPO 4The preparation of buffer solution
Elder generation's compound concentration is the NaH of 100.0mmol/L 2PO 4Solution and concentration are the Na of 100.0mmol/L 2HPO 4Solution mixes both then, regulates pH value to 8.5.
3. the preparation process of blank urine sample and metoprolol and atenolol standard items mark-on urine sample is:
Get healthy people's urine, through 0.22 μ m membrane filtration, with 20 times of secondary water dilutions, as blank urine sample; Metoprolol and atenolol standard items storing solution added to make in the blank urine sample contain metoprolol and atenolol concentration is 2.5 * 10 -6The mark-on urine sample of mol/L.
3. the separation detection of blank urine sample and metoprolol and atenolol standard items mark-on urine sample
Detecting current potential 1.15V; NaH 2PO 4-Na 2HPO 4The electrophoresis buffer concentration is 10.0mmol/L, and pH 3.0; Sample injection time 2s, sample introduction voltage 10kV; Separate high pressure 15kV; 5mMRu (bpy) 3 2+With 100mM NaH 2PO 4-Na 2HPO 4(pH 8.5) join in the detection cell, and the photomultiplier high pressure is 800V.Under this optimal separation testing conditions, obtain the electrophoresis pattern (Fig. 3) of blank urine sample and metoprolol and atenolol standard items mark-on urine sample.
In experimentation,, need kapillary and working electrode are carried out suitable processing for guaranteeing to obtain higher signal response and quite good detecting reappearance.The influence to separation detection after diluting of compositions such as the protein that contains in the urine sample is very little, so the method for requiring no special processing.
Disposal route capillaceous is: kapillary spends the night with the flushing of 0.1mol/L NaOH solution before using for the first time.In experimentation, spend the night with the flushing of 0.1mol/L NaOH solution every day, more respectively with secondary power and water swimming damping fluid flushing capillary column 5min, and then static hairlet capillary column 10min under the separation condition.
The disposal route of working electrode is: 500 μ m Pt dish working electrode is before use at 1.0mol/LH 2SO 4In the solution, in-0.2-1.5V potential range, circulate and sweep, up to the feature cyclic voltammetry curve that obtains the Pt electrode.With working electrode scan round 10-20 week in detection cell buffer solution, sweep interval is 0-1.35V in the experimentation, to remove the electrode surface pollutant, the activation working electrode surface.

Claims (4)

1. the method for capillary electrophoresis electrochemiluminescdetection detection of metoprolol and atenolol, its detect step and condition as follows:
Used apparatus is: internal diameter 25 μ m not coating melt silicon capillary; Diameter 500 μ m Pt coil working electrode, the saturated KCl solution of Ag/AgCl/ contrast electrode, Pt silk auxiliary electrode; MPI-A type capillary electrophoresis electrochemical light-emitting detector;
Agents useful for same is: Ru (bpy) 3Cl 26H 2O, NaH 2PO 4, Na 2HPO 4, H 3PO 4, NaOH, metoprolol and atenolol standard items; It is pure that agents useful for same is analysis; All solution are all with secondary water preparation, the solution for preparing before using all through 0.22 μ m membrane filtration;
1), kapillary and working electrode are done following processing:
(1), kapillary before using for the first time, wash with 0.1mol/L NaOH solution and to spend the night; In operating process, spend the night with the flushing of 0.1mol/L NaOH solution every day, more respectively with secondary power and water swimming damping fluid flushing capillary column 2-10min, balance 2-10min under separation condition at last;
(2), diameter 500 μ m Pt dish working electrode before operation at 1.0mol/L H 2SO 4In the solution, in-0.2-1.5V potential range, circulate and sweep, up to the feature cyclic voltammetry curve that obtains the Pt electrode, in the operating process with working electrode scan round 10-20 week in detection cell buffer solution, the scanning potential range is 0-1.35V, to remove the electrode surface pollutant, the activation working electrode;
2), the preparation of buffer solution
(1), the compound method of the buffer solution of pH＜5.0 is:
Elder generation's compound concentration is the NaH of 10-50mmol/L 2PO 4Solution and concentration are the H of 1.0mol/L 3PO 4Solution is used the H of 1.0mol/L then 3PO 4Solution is adjusted to pH＜5.0;
(2), the compound method of the buffer solution of 5.0≤pH≤9.0 is:
Compound concentration is the NaH of 10-100mmol/L respectively earlier 2PO 4And Na 2HPO 4Solution will can obtain the buffer solution of 5.0≤pH≤9.0 with the two mixing of concentration;
(3), pH〉compound method of 9.0 buffer solution is:
Elder generation's compound concentration is the Na of 10-100mmol/L 2HPO 4With concentration be the NaOH solution of 1.0mol/L, the NaOH solution with 1.0mol/L is adjusted to pH then〉9.0;
3), the preparation of metoprolol and atenolol standard solution and static experiment thereof
The concentration of metoprolol and atenolol storing solution is 1.0mmol/L, and storing solution keeps in Dark Place in 4 ℃ of refrigerators;
The static state experiment of metoprolol and atenolol standard solution:
With 100mmol/L, the NaH of pH7.5 2PO 4-Na 2HPO 4Buffer solution is electrolyte as a setting, and the scanning potential range is 0-1.35V, cyclic voltammetric (CV) curve and electrochemiluminescence (ECL) curve when record is stablized; Scan round in the back-ground electolyte that contains 0.4mmol/L metoprolol and atenolol then, sweep interval is similarly 0-1.35V, CV curve and ECL curve when record is stablized; With the contrast of CV curve and the ECL curve and the back-ground electolyte of metoprolol and atenolol, whether has enhancing Ru (bpy) to determine metoprolol and atenolol 3 2+The electrochemiluminescence activity;
4), the testing conditions of Capillary Zone Electrophoresis with Electrochemical luminous detection metoprolol and atenolol standard solution, and carry out the investigation of the range of linearity and detectability with this understanding
Select the constant potential mode of operation, change-detection current potential between 1.0-1.3V; 2-10s changes sample injection time and sample introduction high pressure between the 10-15kV; Change between the 10-20kV and separate high pressure; 10.0-50.0mmol/L between change NaH 2PO 4-Na 2HPO 4The electrophoresis buffer concentration changes NaH between the 5.0-9.0 2PO 4-Na 2HPO 4The electrophoresis pH value of buffer solution; NaH in the detection cell 2PO 4-Na 2HPO 4Electrophoresis buffer solution is fixed as 100mmol/L, and the pH value changes between 5.0-9.0; Ru in the detection cell (bpy) 3 2+Concentration in the 1.0-10.0mmol/L scope, change; The photomultiplier high pressure is 600-900V;
Under the above-mentioned testing conditions that obtains, 5 * 10 -9-1.0 * 10 -5Investigate the detection range of linearity of metoprolol in the mol/L concentration range; 7.5 * 10 -8-1.0 * 10 -5Investigate the detection range of linearity of atenolol in the mol/L concentration range, also investigated the detection lower limit of the two simultaneously;
5), the investigation of metoprolol and atenolol standard solution separation condition
Sample injection time changes between 1-10s, changes NaH between the 10.0-50.0mmol/L 2PO 4-Na 2HPO 4The electrophoresis buffer concentration changes NaH between the 5.0-9.0 2PO 4-Na 2HPO 4The electrophoresis pH value of buffer solution;
6), blank urine sample and contain metoprolol and the preparation process of the mark-on urine sample of atenolol standard items
Get healthy people's urine, through 0.22 μ m membrane filtration, afterwards doubly with secondary water dilution 10-20, as blank urine sample; Isopyknic metoprolol and atenolol storing solution added to be made in the blank urine sample contain metoprolol and atenolol standard items concentration is 1.0 * 10 -7-1.0 * 10 -5The mark-on urine sample of mol/L;
7), blank urine sample and contain metoprolol and the detection of the mark-on urine sample of atenolol standard items
5) under the optimal separation testing conditions of gained, obtain blank urine sample and contain metoprolol and the electrophoresis pattern of the mark-on urine sample of atenolol standard items.
2, the capillary electrophoresis electrochemical light-emitting detection method of a kind of metoprolol described in claim 1 and atenolol is characterized in that, in the described step 4), the top condition that detects is to detect current potential 1.15V, sample injection time 8s, sample introduction high pressure 10kV, separate high pressure 15kV, NaH 2PO 4-Na 2HPO 4Electrophoresis buffer concentration 10.0mmol/L pH8.5,5mM Ru (bpy) 3 2+With 100mM NaH 2PO 4-Na 2HPO 4PH8.5 joins in the detection cell, and the photomultiplier high pressure is 800V.
3, the capillary electrophoresis electrochemical light-emitting detection method of a kind of metoprolol described in claim 1 and atenolol is characterized in that, in the described step 5), the optimal separation condition of metoprolol and atenolol is 10.0mmol/L NaH 2PO 4-Na 2HPO 4Electrophoresis buffer solution pH3.0,10kV electrokinetic injection 2s.
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CN114486444B (en) * 2022-02-07 2024-02-20 洛阳师范学院 Capillary electrophoresis separation method of atenolol non-racemate mixture

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