CN101788490B - Method for simultaneously carrying out chiral separation analysis on anisodamine, atenolol and metoprolol - Google Patents
Method for simultaneously carrying out chiral separation analysis on anisodamine, atenolol and metoprolol Download PDFInfo
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- CN101788490B CN101788490B CN2010101079101A CN201010107910A CN101788490B CN 101788490 B CN101788490 B CN 101788490B CN 2010101079101 A CN2010101079101 A CN 2010101079101A CN 201010107910 A CN201010107910 A CN 201010107910A CN 101788490 B CN101788490 B CN 101788490B
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Abstract
The invention provides a method for simultaneously carrying out chiral separation analysis on anisodamine, atenolol and metoprolol, which comprises the following steps: putting an anisodamine sample, an atenolol sample and a metoprolol sample in a sample cell of a capillary electrophoresis electrochemistry luminescence detection hyphenated instrument and applying an injection voltage to make the samples enter a capillary of the instrument; applying a separation voltage to make the samples carry out electrophoretic separation in the capillary, wherein the capillary is filled with separation solution comprising carboxymethyl-beta-cyclodextrin and the pH value of the separation solution is between 3.0 and 6.0; and making the separated samples enter a detection cell of the instrument and applying a detection voltage to carry out detection, wherein the detection cell is filled with detection solution comprising tris (bipyridine) ruthenium and the pH value of the detection solution is between 6.0 and 9.0. Compared with the prior art, the method for carrying out chiral separation analysis, which is provided by the invention, has the advantages of less reagent use, lower detection cost, higher separation efficiency and higher detection sensitivity.
Description
Technical field
The present invention relates to the chiral separation analysis field of chiral drug, relate in particular to the method for a kind of while chiral separation analysis anisodamine, atenolol and metoprolol.
Background technology
Atenolol and metoprolol all belong to β 1 adrenoreceptor and suppress a type medicine, have similar structure and character, are widely used in the treatment of angiocardiopathies such as hypertension, angina pectoris, arrhythmia cordis and miocardial infarction.Anisodamine is an anticholinergic agent, the clinical treatment of diseases such as smooth muscle spasm, stomach and intestine angina, biliary tract spasm that are mainly used in.Atenolol, metoprolol and anisodamine are chiral drug; Its enantiomter separately exists than big-difference in pharmacology, toxicity and even clinical properties; Therefore, it is significant atenolol enantiomter, metoprolol enantiomter and anisodamine enantiomter to be carried out compartment analysis.
Prior art discloses the method for multiple chiral separation analysis atenolol, metoprolol and anisodamine; Like usefulness Capillary Electrophoresis ultraviolet detection methods such as H.Wang the anisodamine enantiomter has been carried out separating (H.Wang; J.L.Gu, H.F.Hu, R.J.Dai; T.H.Ding, R.N.Fu.Analytica chimica acta, 1998,359; 39), usefulness Capillary Electrophoresis ultraviolet detection methods such as H.-L.Zhang have carried out separating (H-L.Zhang, H.Shao one by one to the corresponding isomeride of chirality atenolol with the metoprolol tartrate enantiomter; Y-M.A, Z-Z.Zhang.Chromatographia, 2008; 68,653).But uv detection method sensitivity is lower, is difficult to satisfy highly sensitive detection requirement.
Electrochemical luminescence method is a kind of novel analyzing detecting method, and especially with the bipyridyl ruthenium system during as luminescence system, luminescence efficiency is higher, and detection sensitivity is also higher.Prior art discloses uses the capillary electrophoresis electrochemical light-emitting method materials such as amino acid, protein, DNA and organic amine to be carried out the technology of separation detection; The method of a kind of capillary electrophoresis electrochemiluminescdetection detection of metoprolol and atenolol is disclosed like Chinese patent document 200610173390.8; Use capillary electrophoresis electrochemical light-emitting technology has been carried out compartment analysis with the metoprolol and the atenolol of structural similarity, but does not realize the compartment analysis of metoprolol enantiomter and atenolol enantiomter.
Therefore, the inventor considers to provide a kind of method simultaneously anisodamine enantiomter, atenolol enantiomter and metoprolol stage enantiomer separation to be detected, and reducing cost, to raise the efficiency, and obtains higher detection sensitivity.
Summary of the invention
In view of this; Technical matters to be solved by this invention has been to provide the method for a kind of while chiral separation analysis anisodamine, atenolol and metoprolol; Method provided by the invention can reduce the chiral drug separation detection of different structure to detect cost, improves separation efficiency.
The invention provides the method for a kind of while chiral separation analysis anisodamine, atenolol and metoprolol, comprising:
Anisodamine sample, atenolol sample and metoprolol sample are dropped in the sample cell of capillary electrophoresis electrochemical light-emitting detection coupling instrument, apply sample introduction voltage, make said sample get into the kapillary of said instrument;
Apply separation voltage, make said sample in said kapillary, carry out electrophoretic separation, said kapillary is the separation solution that contains carboxymethyl-beta-cyclodextrin, and the pH value of said separation solution is 3.0-6.0;
Sample after the separation gets into the detection cell of said instrument, applies detection voltage and detects, and for containing the detection solution of tris (bipyridine) ruthenium, the pH value of said detection solution is 6.0-9.0 in the said detection cell.
Preferably, the concentration of said carboxymethyl-beta-cyclodextrin is 5mmol/L-20mmol/L.
Preferably, the concentration of said carboxymethyl-beta-cyclodextrin is 13mmol/L-16mmol/L.
Preferably, the pH value of said separation solution is kept by HAc-NaAc buffer solution.
Preferably, the concentration of said HAc-NaAc buffer solution is 30mmol/L-70mmol/L.
Preferably, the concentration of said tris (bipyridine) ruthenium is 4mmol/L-10mmol/L.
Preferably, the concentration of said tris (bipyridine) ruthenium is 5mmol/L.
Preferably, the pH value of said detection solution is by NaH
2PO
4-Na
2HPO
4Buffer solution keeps.
Preferably, said NaH
2PO
4-Na
2HPO
4The concentration of buffer solution is 50mmol/L-150mmol/L.
Preferably, said kapillary is that internal diameter is that the not coating of 50 μ m is melted silicon capillary.
Compared with prior art; The present invention is chiral selector with the carboxymethyl-beta-cyclodextrin; Make the isomeride of anisodamine, atenolol and the metoprolol of different structure be electrophoretic separation in the kapillary of 3.0-6.0 in the pH value; Through the tris (bipyridine) ruthenium electrochemiluminescsystem system each isomeride is detected separation detection when finally realizing then to 3 kinds of chiral drugs such as anisodamine, atenolol and metoprolols.Chiral isolation analysis method reagent use provided by the invention is less, the detection cost is lower, separation efficiency is higher, detection sensitivity is higher.Experiment shows that when simultaneously anisodamine enantiomter, atenolol enantiomter and metoprolol enantiomter being carried out separation detection through method provided by the invention, the detectability of anisodamine, atenolol and metoprolol is respectively 6 * 10
-7Mol/L, 5.5 * 10
-7Mol/L and 3 * 10
-7Mol/L.
Description of drawings
The NaH that Fig. 1 provides for the embodiment of the invention
2PO
4-Na
2HPO
4Buffer solution, tris (bipyridine) ruthenium, anisodamine, atenolol and the metoprolol cyclic voltammetry curve figure on platinum disk electrode;
The NaH that Fig. 2 provides for the embodiment of the invention
2PO
4-Na
2HPO
4The electrochemiluminescence curve map of buffer solution, tris (bipyridine) ruthenium, anisodamine, atenolol and metoprolol;
The electrophoresis spectrogram of the anisodamine that Fig. 3 provides for the embodiment of the invention, atenolol and metoprolol;
Blank urine sample that Fig. 4 provides for the embodiment of the invention and the electrophoresis spectrogram that has added the urine sample of anisodamine, atenolol and metoprolol.
Embodiment
The invention provides the method for a kind of while chiral separation analysis anisodamine, atenolol and metoprolol, comprising:
Anisodamine sample, atenolol sample and metoprolol sample are dropped in the sample cell of capillary electrophoresis electrochemical light-emitting detection coupling instrument, apply sample introduction voltage, make said sample get into the kapillary of said instrument;
Apply separation voltage, make said sample in said kapillary, carry out electrophoretic separation, said kapillary is the separation solution that contains carboxymethyl-beta-cyclodextrin, and the pH value of said separation solution is 3.0-6.0;
Sample after the separation gets into the detection cell of said instrument, applies detection voltage and detects, and for containing the detection solution of tris (bipyridine) ruthenium, the pH value of said detection solution is 6.0-9.0 in the said detection cell.
According to the present invention, at first anisodamine sample, atenolol sample and metoprolol sample are dropped in the sample cell of capillary electrophoresis electrochemical light-emitting detection coupling instrument, apply sample introduction voltage, make said sample get into the kapillary of said instrument.The present invention does not have particular restriction to the source that capillary electrophoresis electrochemical light-emitting detects the coupling instrument, can buy the MPI-A type capillary electrophoresis electrochemical light-emitting detector of selling like the auspicious analytical instrument advanced in years in Xi'an Ltd from market.The present invention does not have particular restriction to sample introduction voltage, is preferably 10kV-20kV, more preferably 10kV-15kV.The present invention does not have particular restriction to employed kapillary, and the not coating that is preferably internal diameter 50 μ m is melted silicon capillary.In order to make the sample separation better effects if, sample injection time of the present invention is preferably 2s-15s, and more preferably 2s-10s most preferably is 3s-8s.For the sensitivity that guarantees to detect and the reappearance of analysis result; Preferably before sample introduction, said kapillary is carried out pre-service; Preferably use the NaOH solution of 80mmol/L-120mmol/L to wash said kapillary 5min-15min successively, secondary water washes said kapillary 2min-6min, 30mmol/L-70mmol/L, pH value wash said kapillary 5min-15min for the HAc-NaAc buffer solution between the 3.0-6.0.
Said sample applies separation voltage to kapillary after getting into kapillary, makes sample in kapillary, realize electrophoretic separation.The present invention does not have particular restriction to said separation voltage, is preferably 10kV-20kV, and more preferably 13kV-20kV most preferably is 13kV-15kV.
It in the said kapillary separation solution that contains carboxymethyl-beta-cyclodextrin.Because with also need in the luminescence system of three pyridine rutheniums, detecting after anisodamine enantiomter, atenolol enantiomter and the metoprolol enantiomter electrophoretic separation; Therefore; The present invention uses the carboxymethyl-beta-cyclodextrin that does not have reductibility as chiral selector, reduces the influence of reagent to the subsequent detection result.Said carboxymethyl-beta-cyclodextrin can combine to form complex compound respectively with anisodamine enantiomter, atenolol enantiomter and metoprolol enantiomter; But the degree of stability of the complex compound that forms is different; Therefore in kapillary, to carry out the speed of electrophoresis also different for said complex compound, thereby finally realize the separation of enantiomter.Experiment shows that the anisodamine enantiomter combines with carboxymethyl-beta-cyclodextrin at first and separates, and the metoprolol enantiomter combines with carboxymethyl-beta-cyclodextrin at last and separates.The present invention does not have particular restriction to the concentration of said carboxymethyl-beta-cyclodextrin, is preferably lmmol/L-25mmol/L, and more preferably 5mmol/L-25mmol/L most preferably is 5mmol/L-20mmol/L.
According to the present invention; The pH value of solution is 3.0-6.0 in the said kapillary; The pH value of said solution is preferably kept by buffer solution, and said buffer solution is preferably HAc-NaAc buffer solution well known to those skilled in the art, and the concentration of said HAc-NaAc is preferably 10mmol/L-100mmol/L; More preferably 20mmol/L-90mmol/L most preferably is 30mmol/L-70mmol/L.
After said anisodamine enantiomter, atenolol enantiomter and metoprolol enantiomter realize separating in kapillary, successively get in the detection cell of capillary electrophoresis electrochemical light-emitting detection coupling instrument, under detection voltage, detect.The present invention does not have particular restriction to detecting voltage, is preferably 1.0V-1.4V, more preferably 1.0V-1.2V.
For containing the solution of tris (bipyridine) ruthenium, said tris (bipyridine) ruthenium is the most common electrochemiluminescsystem system in the said detection cell, and its luminous detection principle is following: contain Ru (bpy) in the terpyridyl ruthenium system
3 2+, Ru (bpy)
3 2+Be oxidized to unsettled oxidation state Ru (bpy) through working electrode
3 3+, this oxidation state material and chirality anisodamine interact, and are reduced into the Ru (bpy) of excited state
3 2+*, this excited state is moved back to ground state Ru (bpy) immediately
3 2+, and discharging photon, the intensity of this light signal and the concentration of measured object are linear.Because anisodamine, atenolol and metoprolol respectively has left-handed and two kinds of isomeride of dextrorotation; Successively get into detection cell through capillary electrophoresis separation; Can successively take place to excite for six times; Produce six peak of luminous intensity, thereby realize detection anisodamine enantiomter, atenolol enantiomter and metoprolol enantiomter.The present invention does not have particular restriction to the concentration of tris (bipyridine) ruthenium, is preferably 1mmol/L-20mmol/L, and more preferably 1mmol/L-15mmol/L most preferably is 4mmol/L-10mmol/L.
According to the present invention, the pH value of solution is 6.0-9.0 in the said detection cell, is preferably kept by buffer solution, and said buffer solution is preferably NaH well known to those skilled in the art
2PO
4-Na
2HPO
4Damping fluid, NaH
2PO
4-Na
2HPO
4The concentration of damping fluid is preferably 10mmol/L-200mmol/L, and more preferably 30mmol/L-200mmol/L most preferably is 50mmol/L-150mmol/L.
According to the present invention, be three-electrode system in the said detection cell, said three-electrode system is preferably: diameter is that the Pt of 500 μ m coils working electrode, Ag/AgCl contrast electrode (KCl saturated solution) and Pt silk to electrode.
According to the present invention; The luminescence detector that said capillary electrophoresis electrochemical light-emitting detects the coupling instrument is used for detecting and the recording light signal; Obtain the spectrogram that kapillary-electrochemiluminescence detects, thereby obtain the chiral separation analysis result of anisodamine, atenolol and metoprolol.According to the present invention, said luminescence detector is preferably photomultiplier, and its voltage is preferably 700V-900V.
According to the present invention, anisodamine, atenolol and metoprolol after preferably will separating carry out structure analysis well known to those skilled in the art, to confirm that the material after the separation is that left-handed molecule still is the dextrorotation molecule.
Compared with prior art; The present invention is chiral selector with the carboxymethyl-beta-cyclodextrin; Make the isomeride of anisodamine, atenolol and the metoprolol of different structure be electrophoretic separation in the kapillary of 3.0-6.0 in the pH value; Through the tris (bipyridine) ruthenium electrochemiluminescsystem system each isomeride is detected chiral separation analysis when finally realizing anisodamine, atenolol and metoprolol then.Chiral isolation analysis method reagent use provided by the invention is less, the detection cost is lower, separation efficiency is higher, detection sensitivity is higher.Experiment shows that when simultaneously anisodamine, atenolol and metoprolol being carried out chiral separation analysis through method provided by the invention, the detectability of anisodamine, atenolol and metoprolol is respectively 6 * 10
-7Mol/L, 5.5 * 10
-7Mol/L and 3 * 10
-7Mol/L.
In order further to understand the present invention, the method for while chiral separation analysis anisodamine provided by the invention, atenolol and metoprolol is described in detail below in conjunction with embodiment.
Prepare NaH according to the following steps
2PO
4-Na
2HPO
4Buffer solution:
Compound concentration is the NaH of 200mmol/L respectively
2PO
4The Na of solution and 200mmol/L
2HPO
4Solution after two solution are mixed, uses secondary water to be diluted to concentration and is 100mmol/L, then the pH of mixed solution is transferred to 7.0 subsequent use.
Prepare HAc-NaAc buffer solution according to following steps:
At first compound concentration is the NaAc solution of 200mmol/L, is diluted to 57.6mmol/L with secondary water then, the pH value of solution is transferred to 5.3 subsequent use with glacial acetic acid then.
Embodiment 3
The apparatus that uses is: the not coating of internal diameter 50 μ m is melted the silicon capillary post; The Pt dish working electrode of diameter 500 μ m; Ag/AgCl contrast electrode, Pt silk be to electrode, the MPI-A type capillary electrophoresis electrochemical light-emitting detector that auspicious analytical instrument advanced in years Ltd buys from Xi'an.
NaH with embodiment 1 preparation
2PO
4-Na
2HPO
4Buffer solution is back-ground electolyte, and the scanning current potential is 0-1.30V, and cyclic voltammetry curve and electrochemiluminescence curve when record is stablized are referring to a curve among Fig. 1 and a curve among Fig. 2;
In said back-ground electolyte, add the tris (bipyridine) ruthenium of 5mmol/L, the scanning current potential is 0-1.30V, and cyclic voltammetry curve and electrochemiluminescence curve when record is stablized are referring to b curve among Fig. 1 and the b curve among Fig. 2;
The anisodamine, the atenolol of 0.3mmol/L and the metoprolol of 0.3mmol/L that in the solution that contains tris (bipyridine) ruthenium, add 0.3mmol/L; The scanning current potential is 0-1.30V; Cyclic voltammetry curve and electrochemiluminescence curve when record is stablized are respectively referring to the c curve among the c curve among Fig. 1, d curve, e curve and Fig. 2, d curve, e curve.
With resulting cyclic voltammetry curve and the contrast of electrochemiluminescence curve, referring to Fig. 1 and Fig. 2, the NaH that Fig. 1 provides for the embodiment of the invention
2PO
4-Na
2HPO
4Buffer solution, tris (bipyridine) ruthenium, anisodamine, atenolol and the metoprolol cyclic voltammetry curve figure on platinum disk electrode; The NaH that Fig. 2 provides for the embodiment of the invention
2PO
4-Na
2HPO
4The electrochemiluminescence curve map of buffer solution, tris (bipyridine) ruthenium, anisodamine, atenolol and metoprolol; Can know that by Fig. 1 behind adding anisodamine, atenolol and the metoprolol, the electroresponse of solution does not significantly strengthen; Can know by Fig. 2; After adding anisodamine, atenolol and metoprolol; Responsiveness in the electrochemiluminescence curve of solution is stronger than the responsiveness that only adds tris (bipyridine) ruthenium, can not strengthen the electrochemical activity of tris (bipyridine) ruthenium though anisodamine, atenolol and metoprolol are described, the electrochemiluminescence that can strengthen tris (bipyridine) ruthenium is active; Therefore, it is feasible using electrochemical luminescence method to detect anisodamine, atenolol and metoprolol simultaneously.
Embodiment 4
The apparatus that uses is: the not coating of internal diameter 50 μ m is melted the silicon capillary post, and the Pt dish working electrode of diameter 500 μ m, Ag/AgCl contrast electrode, Pt silk be to electrode, MPI-A type capillary electrophoresis electrochemical light-emitting detector.
NaH with embodiment 1 preparation
2PO
4-Na
2HPO
4The terpyridyl ruthenium solution of buffer solution and 5mmol/L joins in the detection cell of MPI-A type capillary electrophoresis electrochemical light-emitting detector, and the HAc-NaAc buffer solution of embodiment 2 preparations and the carboxymethyl-beta-cyclodextrin of 14.7mol/L are joined in the kapillary of MPI-A type capillary electrophoresis electrochemical light-emitting detector.
Kapillary is carried out pre-service: at first subsequent use with the NaOH solution flushing back of 100mmol/L; Before use, the flushing of HAc-NaAc buffer solution 10min, 5min and the 10min that prepare with NaOH solution, the secondary WS and the embodiment 2 of 100mmol/L successively again.
The anisodamine solution of 1.0mmol/L, the atenolol solution of 1.0mmol/L and the metoprolol solution of 1.0mmol/L are joined in the sample cell of MPI-A type capillary electrophoresis electrochemical light-emitting detector; The operating conditions of control MPI-A type capillary electrophoresis electrochemical light-emitting detector is following: sample introduction voltage 10kV, sample injection time 4s; Separation voltage 17.5kV; Detect voltage 1.15V; The photomultiplier transit photovoltage is 800V; Anisodamine, atenolol and metoprolol are carried out chiral separation analysis, and testing result is referring to Fig. 3, the electrophoresis spectrogram of the anisodamine that Fig. 3 provides for the embodiment of the invention, atenolol and metoprolol; Can know by Fig. 3, behind the beginning chiral separation analysis, A1, two peaks of A2 occur during 1133s, occur B1, two peaks of B2 during 2489s, occur C1, two peaks of C2 during 3074s.
Keep the chiral separation analysis condition constant; With the anisodamine solution of 2.0mmol/L, the atenolol solution of 1.0mmol/L and the metoprolol solution of 1.0mmol/L is that sample carries out chiral separation analysis; In the electrophoresis spectrogram that obtains; Variation has taken place in the time of occurrence and the peak shape at two peaks that occur at first, but still is to occur at first, and the time of occurrence and the peak shape at four peaks of back have no significant change; Can learn the peak that the A1 that 1133s occurs among Fig. 3 and two peaks of A2 are the anisodamine enantiomter thus.
Keep the chiral separation analysis condition constant; With the anisodamine solution of 1.0mmol/L, the atenolol solution of 2.0mmol/L and the metoprolol solution of 1.0mmol/L is that sample carries out chiral separation analysis; In the electrophoresis spectrogram that obtains; Variation has taken place in the time of occurrence and the peak shape at middle two peaks that occur, but still is to occur in the centre, and the time of occurrence and the peak shape at two peaks in two peaks, front and back have no significant change; Can learn the peak that the B1 that 2489s occurs among Fig. 3 and two peaks of B2 are the atenolol enantiomter thus.
Keep the chiral separation analysis condition constant; With the anisodamine solution of 1.0mmol/L, the atenolol solution of 1.0mmol/L and the metoprolol solution of 2.0mmol/L is that sample carries out chiral separation analysis; In the electrophoresis spectrogram that obtains; Variation has taken place in the time of occurrence and the peak shape at two peaks that occur at last, but still occurs at last, and the time of occurrence and the peak shape at four peaks of front have no significant change; Can learn the peak that the C1 that 3074s occurs among Fig. 3 and two peaks of C2 are the metoprolol enantiomter thus.
Hence one can see that, and anisodamine, atenolol and metoprolol and tris (bipyridine) ruthenium are had an effect and discharged the asynchronism(-nization) of photon, and therefore, method provided by the invention can be carried out chiral separation analysis with anisodamine, atenolol and metoprolol simultaneously.
Under the aforesaid operations condition, the detection limit of anisodamine, atenolol and metoprolol is respectively 6 * 10
-7Mol/L, 5.5 * 10
-7Mol/L and 3 * 10
-7Mol/L.
Embodiment 5
Get the urine of healthy subjects, behind 0.22 μ m membrane filtration, the buffer solution for preparing with embodiment 2 dilutes it, as blank urine sample; In blank urine sample, add 6 * 10
-5The anisodamine solution, 5.0 * 10 of mol/L
-5The atenolol solution and 3 * 10 of mol/L
-5The metoprolol solution of mol/L.
Use instrument, reagent and the operating conditions identical that the blank urine sample and the urine sample of having added chiral drug are carried out chiral separation analysis with embodiment 4; The result is referring to Fig. 4, blank urine sample that Fig. 4 provides for the embodiment of the invention and the electrophoresis spectrogram that has added the urine sample of anisodamine, atenolol and metoprolol.Among Fig. 4, curve 1 is the electrophoresis spectrogram of blank urine sample, and curve 2 is the electrophoresis spectrogram that has added the urine sample of anisodamine, atenolol and metoprolol; In curve 2; A1 and two peaks of A2 have appearred in the 1133s place, and B1 and two peaks of B2 have appearred in the 2489s place, and C1 and two peaks of C2 have appearred in the 3074s place.
The analysis of reference implementation example 4, A1 and A2 are the peak of anisodamine isomers, and B1 and B2 are respectively the peak of atenolol isomers, and C1 and C2 are respectively the peak of metoprolol isomers.This shows that the substrate of urine is to the not very big influence of separation of these three kinds of chiral materials, method provided by the invention can realize the anisodamine in the urine, atenolol and metoprolol are carried out chiral separation analysis simultaneously.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (10)
1. the method for a while chiral separation analysis anisodamine, atenolol and metoprolol is characterized in that, comprising:
Anisodamine sample, atenolol sample and metoprolol sample are dropped in the sample cell of capillary electrophoresis electrochemical light-emitting detection coupling instrument, apply sample introduction voltage, make said sample get into the kapillary of said instrument;
Apply separation voltage, make said sample in said kapillary, carry out electrophoretic separation, have the separation solution that contains carboxymethyl-beta-cyclodextrin in the said kapillary, the pH value of said separation solution is 3.0-6.0;
Sample after the separation gets into the detection cell of said instrument, applies detection voltage and detects, and has the detection solution that contains tris (bipyridine) ruthenium in the said detection cell, and the pH value of said detection solution is 6.0-9.0.
2. method according to claim 1 is characterized in that, the concentration of said carboxymethyl-beta-cyclodextrin is 5mmol/L-20mmol/L.
3. method according to claim 2 is characterized in that, the concentration of said carboxymethyl-beta-cyclodextrin is 13mmol/L-16mmol/L.
4. method according to claim 1 is characterized in that, the pH value of said separation solution is kept by HAc-NaAc buffer solution.
5. method according to claim 4 is characterized in that, the concentration of said HAc-NaAc buffer solution is 30mmol/L-70mmol/L.
6. method according to claim 1 is characterized in that, the concentration of said tris (bipyridine) ruthenium is 4mmol/L-10mmol/L.
7. method according to claim 1 is characterized in that, the concentration of said tris (bipyridine) ruthenium is 5mmol/L.
8. method according to claim 1 is characterized in that, the pH value of said detection solution is by NaH
2PO
4-Na
2HPO
4Buffer solution keeps.
9. method according to claim 8 is characterized in that, said NaH
2PO
4-Na
2HPO
4The concentration of buffer solution is 50mmol/L-150mmol/L.
10. method according to claim 1 is characterized in that, said kapillary is that internal diameter is that the not coating of 50 μ m is melted silicon capillary.
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| CN112010724B (en) * | 2020-09-04 | 2023-09-08 | 南京师范大学常州创新发展研究院 | Naphthalene derivative isomer separation and cyclodextrin binding constant determination method |
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|---|---|---|---|---|
| CN1995983A (en) * | 2006-12-29 | 2007-07-11 | 中国科学院长春应用化学研究所 | Method for capillary electrophoresis electrochemiluminescence detection of metoprolol and atenolol |
| CN101349647A (en) * | 2008-08-29 | 2009-01-21 | 福州大学 | Novel capillary electrophoresis electrochemical luminescence testing device and use method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1995983A (en) * | 2006-12-29 | 2007-07-11 | 中国科学院长春应用化学研究所 | Method for capillary electrophoresis electrochemiluminescence detection of metoprolol and atenolol |
| CN101349647A (en) * | 2008-08-29 | 2009-01-21 | 福州大学 | Novel capillary electrophoresis electrochemical luminescence testing device and use method thereof |
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| Title |
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| Baiqing Yuan et al..Simultaneous determination of atropine, anisodamine, and scopolamine in plant extract by nonaqueous capillary electrophoresis coupled with electrochemiluminescence and electrochemistry dual detection.《Journal of Chromatography A》.2010,第1217卷(第1期),第171-174页. * |
| JP特开2004-77276A 2004.03.11 |
| 周兴旺等.毛细管电泳-电致化学发光法测定阿替洛尔.《分析科学学报》.2007,第23卷(第1期),第30-32页. * |
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