CN1773272A - A test bar and its preparing process, and method for synchronous detecting rutin and vitamin C in medicine with the same testing bar - Google Patents
A test bar and its preparing process, and method for synchronous detecting rutin and vitamin C in medicine with the same testing bar Download PDFInfo
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- CN1773272A CN1773272A CN 200510110264 CN200510110264A CN1773272A CN 1773272 A CN1773272 A CN 1773272A CN 200510110264 CN200510110264 CN 200510110264 CN 200510110264 A CN200510110264 A CN 200510110264A CN 1773272 A CN1773272 A CN 1773272A
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Abstract
The present invention relates to a test strip, its preparation method and method for simultaneously detecting rutin and vitamin C in the medicine by using said test strip. Said test strip is formed from a gold matrix electrode and a layer of amino-ethanethiol modified on the gold matrix electrode. Said invention also provides the concrete steps of its preparation method and the action principle of said test strip.
Description
Technical field
The present invention relates to the drug test technical field, the test-strips of heterogeneity content in particularly a kind of detection of drugs simultaneously; The invention also discloses the preparation method of this test-strips, and utilize rutin and ascorbic method in this test-strips while detection of drugs.
Background technology
Rutin mainly is present in the stem and leaf of various plants, is the effective constituent in the Chinese herbal medicine, and its principal ingredient is a flavone compound.
The compound rutin sheet belongs to vitamin medicaments, and its principal ingredient is that (Ascorbic acid AA), is used for the supplemental treatment of high blood pressure clinically for rutin (Rutin) and ascorbic acid.Rutin is a kind of flavonoids of biologically active, has oxidation resistant effect in vivo, medically generally is used for keeping VAR, reduces its permeability, reduces fragility and anti-inflammatory, antiviral etc.
At present, rutin and ascorbic mensuration mostly adopt spectroscopic methodology and liquid phase chromatography.As publication number is in disclosed a kind of Chinese and Western medicine compound preparation of CN1562096A and preparation method thereof, and rutin in its preparation and vitamin C adopt liquid phase chromatography to measure their content.Chromatographic column is easily polluted, the price problem of higher but high performance liquid chromatography then exists.
Ultraviolet spectroscopy is because of the characteristic absorption peak 243 of ascorbic acid, and the characteristic absorption peak 260nm of 267nm and rutin is close, thereby, can't detect simultaneously.Have to adopt to add aluminium salt, form the method that complex compound improves detection sensitivity earlier thereby make.But, must adopt alignment technique could eliminate interference owing to exist other multiple interfering material easily to produce background absorption in the sample.
In addition, bibliographical information heat drop solution is arranged also, the enzymatic degradation method, direct ultraviolet line irradiation, copper ion destroy method etc. are eliminated and are disturbed.Yet the strictness of enzyme process requirement for experiment condition needs 30 degree insulations 30 minutes; Hot and ultraviolet destroy method speed is too slow; The copper ion method need be heated to the 50 ℃ of influences that could eliminate citric acid down in advance.In a word, these operations are loaded down with trivial details, are difficult for practical application and promote.
Recently, the report that has report to measure with Capillary Electrophoresis and ampere method coupling technique, but still need earlier ascorbic acid and rutin after separating, on-line determination.And because use ten thousand volts of high-voltage power supplies, electric current is far longer than the detection signal electric current in the high tension loop, as long as there is the sub-fraction shunting will detect less than marking current, therefore, it is how to overcome the interference of electric current to detecting in the high tension loop that capillary electrophoresis amperometric detects the subject matter that faces, though it is can adopt interface arrangement to reduce this influence, but still undesirable.The interface just because of interface arrangement need be reformed when changing kapillary, it makes trouble, and prolongation analysis time, and interface easily produces bubble and makes the kapillary obstruction.As seen, preparation difference capillaceous, the electric current in the high tension loop produces heat, all can influence test, causes the poor reproducibility of experiment.The used instrument of another big problem experiment complicated and and expensive (also wanting about 100,000 RMB of initial stage overlapped in own assembling one, and tens0000 USD are then wanted in import), also higher to tester's requirement.
Recently, the report that adopts the Direct Electrochemistry method to measure in addition, to have equipment simple though detect when the Direct Electrochemistry method is carried out rutin and ascorbic acid, and sense cycle is short, advantages such as processing ease, thereby have broad application prospects.And miniaturization easily, the exploitation of portable instrument, with low cost, industrialization is convenient.The subject matter of its existence is that rutin is close with the oxidizing potential of ascorbic acid on conventional electrodes.The DPV test of carrying out on naked gold electrode by the mixed solution to rutin and AA also clearly illustrates, the oxidation peak of rutin and AA occurs overlapping, and rutin is earlier oxidized and semiquinone that produce is easy to be restored by AA, i.e. oxidation to AA has catalytic action, thereby disturbs the mensuration of rutin.On the other hand, itself also adsorbs rutin on gold electrode easily, and response current is reduced.These phenomenons have all limited it and have been applied to rutin and ascorbic mensuration simultaneously.
Summary of the invention
Technical matters to be solved by this invention provides a kind of without separation on the one hand, in the time of to rutin and ascorbic acid coexistence system, the test-strips of fast detecting, this test-strips shows by electro-chemical test, and ascorbic acid is at the negative 300mV that moved on the naked gold electrode of the oxidizing potential on this modified electrode; Simultaneously, the oxidizing potential of rutin on modified electrode do not have remarkable change, but response current increases to some extent.
Technical matters to be solved by this invention provides a kind of preparation method of above-mentioned test-strips on the other hand.
Further aspect of the present invention provides a kind of rutin and ascorbic method in this test-strips while detection of drugs of utilizing.
The technical matters that the present invention solves can be achieved through the following technical solutions.
In a first aspect of the present invention, the test-strips that provides is made of the aminoothyl mercaptan that an auri body electrode and one deck adopt the molecular self-assembled monolayer technology to be modified on the auri body electrode.
Above-mentioned aminoothyl mercaptan is preferably the 2-aminoothyl mercaptan.
In a second aspect of the present invention, the preparation method of this test-strips that provides has following steps:
A, polishing, polishing also clean auri body electrode surface with ultrapure water;
B, cleaning auri body electrode water drip washing later are placed on H
2SO
4Carrying out cyclic voltammetry scan in the solution in the potential range of-0.2～1.5V handles;
C, place 2-aminoothyl mercaptan aqueous solution to carry out self assembly at the auri body electrode of handling well, self assembly finishes, and take out the back, the water ultrasonic cleaning, again with getting final product behind the water wash.
In a third aspect of the present invention, what provide utilizes this test-strips rutin and ascorbic method in the detection of drugs simultaneously, it adopts electrochemical measuring method, use three-electrode system, wherein, auri body electrode and the gold electrode of modifying through the aminoothyl mercaptan self-assembled film thereof are working electrode, and saturated calomel electrode is a contrast electrode, and the platinized platinum electrode is an auxiliary electrode; With the pH=7.0 phosphate buffer solution is end liquid, and the compound rutin sample solution of configuration is a test solution, writes down corresponding differential pulse voltammogram (DPV), measures rutin and ascorbic content in the medicine with this.
The present invention uses molecular self-assembled monolayer (Self-assemble monolayer, SAM) technology is modified aminoothyl mercaptan on auri body examination strip, utilize the lotus electropositivity of aminoothyl mercaptan in pH neutral solution, significantly negative moving taking place on than bare electrode on the modified electrode in the oxidizing potential that makes ascorbic acid, move about 300mV as negative, and meanwhile, the current potential of rutin is almost constant, thereby makes the oxidation peak current potential of ascorbic acid separate mutually with the oxidizing potential of rutin.But the oxidation current on modified electrode obviously increases, and utilizes the differentiated pulse voltammetry (Differential Pulse Voltammetry DPV) realizes the purpose of Direct Electrochemistry method, measures rutin and ascorbic content in the medicine simultaneously thereby reach.
Detect when the present invention utilizes the differentiated pulse voltammetry to carry out rutin and ascorbic acid, increased detection sensitivity.Golden little dish base electrode with the processing of microelectronics planar technique is a working electrode, and platinum electrode can be realized detection easy and simple to handle, that sample size is few, highly sensitive for the test-strips of contrast electrode that electrode is held concurrently;
Utilize technology of the present invention, and the base length of appropriate change mercaptan or charged character, when realizing some other medicine, the test-strips that molecular self-assembled monolayer is modified detects.
Description of drawings
Fig. 1 sweeps the speed CV figure of rutin on modified electrode down for difference of the present invention, and wherein illustration is oxidation peak current and the subduplicate graph of a relation of sweeping speed;
Fig. 2 is the DPV figure of rutin on modified electrode of variable concentrations, and wherein illustration is the graph of a relation of oxidation peak current and concentration;
Fig. 3 schemes at modified electrode DPV for the ascorbic acid of Rutin of the present invention and variable concentrations.
Embodiment
Main agents has aminoothyl mercaptan (Adrich company), compound rutin sheet (Shanghai Fosun Zhaohui Pharmaceutical Co., Ltd.) in the following embodiment.It is pure that all the other reagent are all analysis; Research solution is all used ultrapure water (the U.S. Thunder God in Shanghai department Superpure water machine) preparation.Logical nitrogen deoxygenation in the experiment, and keep under the blanket of nitrogen and test.
A kind of test-strips comprises that the aminoothyl mercaptan that an auri body electrode and one deck adopt the molecular self-assembled monolayer technology to be modified on the auri body electrode constitutes.Wherein auri body electrode employing φ is the golden disk electrode of 2mm, and aminoothyl mercaptan adopts the 2-aminoothyl mercaptan.
The preparation method of this test-strips polishes golden disk electrode earlier on abrasive paper for metallograph, use the Al of 0.3,0.05 μ m more successively
2O
3The powder polishing.Then, use the ultrapure water ultrasonic cleaning, take out the back and be placed on 0.5mol/L H with water wash
2SO
4In the potential range of-0.2～1.5V, carry out cyclic voltammetry scan (10V/s sweeps under the speed about about 10 minutes) in the solution.Place 5mmol/L aminoothyl mercaptan aqueous solution to carry out self assembly at the electrode of handling well, taking-up, water ultrasonic cleaning 5min behind the 1h are again with standby behind the water wash.
Utilize rutin and ascorbic method in this test-strips while detection of drugs, be specially:
1, the preparation of sample and test
Accurately take by weighing 5 of compound rutins, be ground into fine powder with mortar and be placed in the mixed liquor (volume 1: 1) of the phosphate buffer solution of ethanol and pH=7, ultrasonic hydrotropy 5min, through filter paper filtering, constant volume promptly gets the compound rutin sample solution in the 50mL volumetric flask.
Phosphate buffer solution with pH=7.0 is an end liquid, the golden disk electrode of modifying with aminoothyl mercaptan is a working electrode, write down corresponding cyclic voltammogram (CV) (referring to Fig. 1) and differential pulse voltammogram (referring to Fig. 2) (DPV, experiment parameter: sweep speed: 4mV/s, pulse potential: 50mV, pulse width: 0.05s, the recurrence interval: 0.2s).
2, the DPV method is directly measured rutin content
In order to improve detection sensitivity, under selected condition determination, measured the current-responsive of variable concentrations rutin with the DPV method.When the concentration range of rutin during at 8～243 μ mol/L, the concentration of peak current and rutin is linear, and regression equation is Ip (μ A)=0.0225 * C
Rutin(μ mol/L) detects and is limited to 6 μ mol/L, correlation coefficient r=0.9923.
Fig. 3 is the fixing concentration of rutin, and the AA that adds variable concentrations carries out interference test.The result shows that peak current increases with the increase of AA concentration on the SAM modified electrode, but the peak current of rutin does not have obvious variation, shows that available this modified electrode carries out the direct mensuration of rutin.
3, the mensuration of sample and recovery test thereof
Draw 3 duplicate samples solution, every part of 1mL, measures respectively according to above-mentioned experiment condition in the 50mL volumetric flask with the buffer solution constant volume.
Draw 3 duplicate samples solution, every part of 1mL adds 5mmol/L rutin standard solution 1mL respectively, in the 50mL volumetric flask, carries out recovery test according to above-mentioned experiment condition with the buffer solution constant volume.
Test result is shown in table 1:
Table 1 rutin sample analysis result (n=3)
| Sample | The sign value | Measured value | The recovery |
| Rutin | 20 | 18(3.5) | 99(2.5) |
In addition, experiment showed, the auxiliary material dextrin in the tablet, starch etc. are interference measurement not also.
Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after having read above-mentioned teachings of the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Claims (10)
1, a kind of test-strips is characterized in that: the aminoothyl mercaptan that adopts the molecular self-assembled monolayer technology to be modified on the auri body electrode by an auri body electrode and one deck constitutes.
2, test-strips according to claim 1 is characterized in that: described aminoothyl mercaptan is the 2-aminoothyl mercaptan.
3, test-strips according to claim 1 is characterized in that: described auri body electrode is the golden disk electrode of diameter phi 2mm.
4, a kind of method for preparing the described test-strips of claim 1 is characterized in that: have following steps:
A, polishing, polishing also clean auri body electrode surface with ultrapure water;
B, cleaning auri body electrode water drip washing later are placed on H
2SO
4Carrying out cyclic voltammetry scan in the solution in the potential range of-0.2～1.5V handles;
C, place the aminoothyl mercaptan aqueous solution to carry out self assembly at the auri body electrode of handling well, self assembly finishes, and take out the back, the water ultrasonic cleaning, again with getting final product behind the water wash.
5, method according to claim 4 is characterized in that: adopt the abrasive paper for metallograph polishing.
6, method according to claim 4 is characterized in that: the Al that adopts 0.3-0.05 μ m
2O
3The powder polishing.
7, method according to claim 4 is characterized in that: described H
2SO
4The concentration of solution is 0.5mol/L.
8, method according to claim 4 is characterized in that: the speed of cyclic voltammetry scan is 10V/s, and the time is 10 minutes.
9, method according to claim 4 is characterized in that: the concentration of described aminoothyl mercaptan aqueous solution is 5mmol/L
10, a kind of described test-strips of claim 1 rutin and ascorbic method in the detection of drugs simultaneously utilized, it is characterized in that: adopt electrochemical measuring method, use three-electrode system, wherein, auri body electrode and the gold electrode of modifying through the aminoothyl mercaptan self-assembled film thereof are working electrode, saturated calomel electrode is a contrast electrode, and the platinized platinum electrode is an auxiliary electrode; Phosphate buffer solution with pH=7.0 is an end liquid, and the compound rutin sample solution of configuration is a test solution, writes down corresponding differential pulse voltammogram, measures rutin and ascorbic content in the medicine with this.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288669A (en) * | 2011-05-04 | 2011-12-21 | 青岛大学 | Electrochemical method based on graphene-modified electrode for simultaneous determination of rutin and quercetin |
| CN104914147A (en) * | 2015-05-25 | 2015-09-16 | 遵义师范学院 | Preparation method and application of magnetic nano-NiFe2O4 based electrochemical sensor |
| CN109916974A (en) * | 2019-03-19 | 2019-06-21 | 辽宁大学 | A kind of electrochemical detection method of quick measurement quinine content and its application |
| CN109975378A (en) * | 2019-04-16 | 2019-07-05 | 武汉科技大学 | The method for constructing Protein tau content detection system in Alzheimer disease blood |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AUPN366995A0 (en) * | 1995-06-20 | 1995-07-13 | Australian Membrane And Biotechnology Research Institute | Self-assembly of bilayer membrane sensors |
| CN1101253C (en) * | 1998-08-25 | 2003-02-12 | 中国科学院长春应用化学研究所 | Single-layer and multilayer molecular assembly system of polyoxometallate |
| US6716577B1 (en) * | 2000-02-02 | 2004-04-06 | Lifescan, Inc. | Electrochemical test strip for use in analyte determination |
| CN1172178C (en) * | 2001-02-16 | 2004-10-20 | 中国科学院长春应用化学研究所 | Method for testing quality of acanthopanax leaf |
| CN1141572C (en) * | 2001-12-12 | 2004-03-10 | 中国科学院长春光学精密机械与物理研究所 | Preparation of electrochemica biological sensor electrode for detecting bacteria |
| GB0215987D0 (en) * | 2002-07-10 | 2002-08-21 | Isis Innovation | Sensor for anions |
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2005
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288669A (en) * | 2011-05-04 | 2011-12-21 | 青岛大学 | Electrochemical method based on graphene-modified electrode for simultaneous determination of rutin and quercetin |
| CN102288669B (en) * | 2011-05-04 | 2013-06-26 | 青岛大学 | Electrochemical method based on graphene-modified electrode for simultaneous determination of rutin and quercetin |
| CN104914147A (en) * | 2015-05-25 | 2015-09-16 | 遵义师范学院 | Preparation method and application of magnetic nano-NiFe2O4 based electrochemical sensor |
| CN109916974A (en) * | 2019-03-19 | 2019-06-21 | 辽宁大学 | A kind of electrochemical detection method of quick measurement quinine content and its application |
| CN109975378A (en) * | 2019-04-16 | 2019-07-05 | 武汉科技大学 | The method for constructing Protein tau content detection system in Alzheimer disease blood |
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