CN105738444A - Preparation method of altretamine molecularly printed electrochemical sensor - Google Patents
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Abstract
The invention discloses a preparation method of an altretamine molecularly printed electrochemical sensor. The preparation method is characterized by comprising the following steps of: firstly, modifying a glassy carbon electrode with a silane coupling agent and nano-gold; in a reactor, adding the following components in percentage by mass: 56%-66% of ethanol, 5%-10% of rosin, 5%-10% of maleic anhydride, 8%-14% of ethylene glycol diacrylate, 8%-14% of chloropropene, 0.5%-2.0% of dimethyl azobisisobutyrate, and 1.5%-3.0% of altretamine to obtain altretamine molecularly printed polymer sol; coating the modified electrode with the polymer; and removing template molecules to obtain the altretamine molecularly printed electrochemical sensor. The sensor has a relatively high identification property on the altretamine, and has the advantages of low cost, high sensitivity, good specificity, rapidness in detection and reusability; the response on the altretamine by the molecularly printed sensor is greatly improved.
Description
Technical field
The present invention relates to the preparation method of a kind of molecular engram sensor and quickly detect applied technical field, particularly toOneThe preparation method planting altretamine molecular imprinting electrochemical sensor, specifically based on molecular engram specific recognition effect, for detecting the altretamine technology in medicine, biological sample.
Background technology
Altretamine (HMM) is a kind of new anticarcinogen, has broad spectrum anticancer activity.Chemical constitution and alkylating agent triethylenemelamine (TEM) with.Its difference is in that the vinyl in replacing TEM to divide with two Mes.But model of action is different, it act as a kind of pyrimidines antimetabolic medicine, it is suppressed that dihydrofolate reductase, it is suppressed that thymine and uracil participates in DNA and RNA.For S phase cycle-specific agent, with cisplatin and alkylating agent without crossing drug resistant.Many animals tumor is all had obvious inhibiting effect by this product, and repeatability is strong.Clinical research in recent years finds, ovarian cancer, pulmonary carcinoma, breast carcinoma, malignant lymphoma are had the curative effect of affirmative by it, particularly in the research to advanced ovarian cancer, due to its toxic and side effects is little and and the antitumor drug such as alkylating agent between without features such as cross-resistances, therefore raising curative effect can be share with other chemotherapeutics, thus there is good clinical value.Altretamine and capsule thereof are " Chinese Pharmacopoeia 2005 version and American Pharmacopeia version are all recorded, content assaying method respectively non-aqueous titration and high performance liquid chromatography.Guideline according to Chinese Pharmacopoeia version revision in 2010, accuracy and the susceptiveness tool of nonaquepous tration method are had a certain impact by the adjuvant considered in preparation, establish the content of the strong high effective liquid chromatography for measuring altretamine capsule of specificity, the method also can separate the impurity in altretamine raw material preferably, through test, the method is quick, accurate, sensitive.But the expensive equipment that high performance liquid chromatography uses, in experimentation, consumptive material price is high, it is necessary to very technical professional's operation, the cycle of mensuration is also long, and high performance liquid chromatography popularity rate is not high.Therefore, setting up the detection method that a kind of selectivity is good, highly sensitive, easy and simple to handle, expense is low, the content tool for detecting altretamine is of great significance.
Molecular imprinting is the emerging technology of the molecular recognition material prepared and have specific selectivity and affinity, and demonstrates good development and application prospect with its precordainment, specific recognition and the extensive big distinguishing feature of practicality three at numerous areas such as chromatographic isolation, Solid-Phase Extraction, bionical sensing, membrance separation.One of current exploitation main method of high selectivity material with molecular recognition function, it is by forming a highly cross-linked rigid macromolecule around template molecule, in the network structure of molecularly imprinted polymer, leave the recognition site with binding ability after removing template molecule, template molecule is shown the high a kind of technology selecting recognition performance.This technology increasingly receives the concern of people with its structure effect precordainment and specific recognition.
According to molecular imprinting electrochemical sensor prepared by this technology, it is applied to pharmaceutical analysis, life science play a very important role.Functional molecular is modified on electrode in a suitable manner, prepares that selectivity is good, highly sensitive, have certain service life reproducible electrochemical sensor to become the problem that analysis science worker makes great efforts to explore.But the blotting membrane thickness prepared by traditional immunoblot method is difficult to control to, high-crosslinking-degree makes electron transmission speed and low-response, Monitoring lower-cut is high and regenerates and poorly reversible, affects molecular imprinting application in electrochemical sensor.Therefore, set up a kind of sensitive, quick, easy, specificity is high, the reproducible economic detection method used, to research worker, manufacturing enterprise, Quality Control personnel, government administration section etc. in the urgent need to, altretamine content accurate quantitative analysis in medicine, biological sample is measured very necessary, altretamine is produced and pharmacological research also has great importance.
Summary of the invention
It is an object of the invention to combine molecular engram with electrochemical sensor, it is provided thatOneThe preparation method planting altretamine molecular imprinting electrochemical sensor, mainly with altretamine for template, the modification of γ-(methacryloxypropyl) propyl trimethoxy silicane, nano Au particle is passed through in glassy carbon electrode surface, improve the sensitivity of sensor, adopt drop-coating to prepare altretamine molecular imprinting electrochemical sensor.
Instrument and reagent
CHI660B electrochemical workstation (Shanghai Chen Hua instrument company), experiment adopts three-electrode system: platinum electrode is auxiliary electrode, and Ag/AgCl is reference electrode (SCE), and glass-carbon electrode (GCE) is working electrode；KQ-250E type ultrasonic cleaner；
Methacryloyloxypropyl methyl diethoxy silane, dehydrated alcohol, ethylene glycol diacrylate, chlorine propylene, Colophonium, maleic anhydride, azo-bis-iso-dimethyl, altretamine；Gold chloride, sodium citrate, phosphate buffer solution；Agents useful for same is analytical pure, and experimental water is redistilled water.
The purpose of the present invention is achieved through the following technical solutions.
OneThe preparation method planting altretamine molecular imprinting electrochemical sensor, it is characterised in that the method has following processing step:
(1) pretreatment of glassy carbon electrode: by the Cr of glass-carbon electrode 0.01 ~ 0.05 μm2O3Powder carries out surface finish, then redistilled water ultrasonic cleaning is used, again with absolute ethanol washing for several times, drying up with nitrogen, be immersed in by electrode containing in the ethanol solution of the methacryloyloxypropyl methyl diethoxy silane that mass percentage concentration is 35 ~ 40%, temperature rises to 60 ± 2 DEG C and soaks 100 ~ 120min, after taking-up, with absolute ethanol washing for several times, dry, obtain pretreatment glass-carbon electrode；
(2) preparation of In Glassy Carbon Electrode Modified With Nano-gold: pretreatment glass-carbon electrode is put in 0.25mol/L aqueous solution of chloraurate, 4 ~ 6h is soaked under room temperature, with deionized water wash after taking-up, place into immersion 2h in the sodium citrate solution that mass percentage concentration is 20 ~ 25%, with deionized water wash after taking-up, natural drying, obtains In Glassy Carbon Electrode Modified With Nano-gold；
(3) preparation of altretamine molecularly imprinted polymer: in the reactor, add by following composition mass percentage concentration, ethanol: 56 ~ 66%, Colophonium: 5 ~ 10%, maleic anhydride: 5 ~ 10%, ethylene glycol diacrylate: 8 ~ 14%, chloropropene: 8 ~ 14%, azo-bis-iso-dimethyl: 0.5 ~ 2.0%, altretamine: 1.5 ~ 3.0%, each constituent content sum is absolutely, stirring and dissolving, logical noble gas deoxygenation 5min, atmosphere of inert gases, temperature rises to 75 ± 2 DEG C of stirring reaction 10 ~ 12h, obtains altretamine molecularly imprinted polymer colloidal sol；
(4) preparation method of altretamine molecular imprinting electrochemical sensor: take altretamine molecularly imprinted polymer colloidal sol 4 ~ 6 μ L and be added drop-wise on In Glassy Carbon Electrode Modified With Nano-gold, it is placed under infrared lamp, volatilize after dry solvent, used the mixed solution immersion 6 ~ 8h of ethanol and hydrochloric acid, remove the template molecule on electrode, with deionized water wash, natural drying, obtain altretamine molecular imprinting electrochemical sensor.
Atmosphere of inert gases described in step (3) passes into until reaction terminates for logical noble gas always.
Noble gas described in step (3) is neon or argon.
The mass ratio of the Colophonium described in step (3) and maleic anhydride is 1:1.
The volume ratio of the ethanol described in step (4) and hydrochloric acid mixed solution is 20:1.
Advantages of the present invention and effect be:
Engram technology, LBL self-assembly method and drop-coating are combined by the present invention, glass-carbon electrode is connected decorated by nano-gold at electrode surface by silane coupler, it is made to improve electric conductivity, drop coating molecularly imprinted polymer on the basis of nanometer gold again, successfully have developed a kind of trace electrochemical sensor with specific selectivity.By comparing with that the response of molecular engram electrode without decorated by nano-gold, the response signal of altretamine molecular imprinting electrochemical sensor prepared by the present invention is greatly improved.Altretamine is shown higher affinity, susceptiveness and selectivity by this trace sensor, and the concentration of response current and altretamine is 1.2 × 10-8~8.0×10-5In good linear relationship within the scope of mol/L, detection is limited to 1.06 × 10-8The altretamine molecular imprinting electrochemical sensor that the present invention is prepared by mol/L is used successfully in medicine, biological sample in the detection of altretamine, the response rate is between 96.26 ~ 104.32%, and the molecular engram sensor that therefore prepared by the present invention can be widely applied to the association area such as chemical industry, biological medicine detection.
Detailed description of the invention
Embodiment 1
(1) pretreatment of glassy carbon electrode: by the Cr of glass-carbon electrode 0.01 ~ 0.05 μm2O3Powder carries out surface finish, then redistilled water ultrasonic cleaning is used, again with absolute ethanol washing for several times, drying up with nitrogen, be immersed in by electrode containing in the ethanol solution of the methacryloyloxypropyl methyl diethoxy silane that mass percentage concentration is 38%, temperature rises to 60 ± 2 DEG C and soaks 110min, after taking-up, with absolute ethanol washing for several times, dry, obtain pretreatment glass-carbon electrode；
(2) preparation of In Glassy Carbon Electrode Modified With Nano-gold: pretreatment glass-carbon electrode is put in 0.25mol/L aqueous solution of chloraurate, 5h is soaked under room temperature, with deionized water wash after taking-up, place into immersion 2h in the sodium citrate solution that mass percentage concentration is 22%, with deionized water wash after taking-up, natural drying, obtains In Glassy Carbon Electrode Modified With Nano-gold；
(3) preparation of altretamine molecularly imprinted polymer: in the reactor, be separately added into, ethanol: 77mL, Colophonium: 8g, maleic anhydride: 8g, ethylene glycol diacrylate: 9.5mL, chloropropene: 12mL, azo-bis-iso-dimethyl: 1.0g, altretamine: 2.0g, stirring and dissolving, logical noble gas deoxygenation 5min, atmosphere of inert gases, temperature rises to 75 ± 2 DEG C of stirring reaction 11h, obtains altretamine molecularly imprinted polymer colloidal sol；
(4) preparation method of altretamine molecular imprinting electrochemical sensor: take altretamine molecularly imprinted polymer colloidal sol 5 μ L and be added drop-wise on In Glassy Carbon Electrode Modified With Nano-gold, it is placed under infrared lamp, volatilize after dry solvent, used the mixed solution immersion 7h of ethanol and hydrochloric acid, remove the template molecule on electrode, with deionized water wash, natural drying, obtain altretamine molecular imprinting electrochemical sensor.
Embodiment 2
(1) pretreatment of glassy carbon electrode: by the Cr of glass-carbon electrode 0.01 ~ 0.05 μm2O3Powder carries out surface finish, then redistilled water ultrasonic cleaning is used, again with absolute ethanol washing for several times, drying up with nitrogen, be immersed in by electrode containing in the ethanol solution of the methacryloyloxypropyl methyl diethoxy silane that mass percentage concentration is 35%, temperature rises to 60 ± 2 DEG C and soaks 120min, after taking-up, with absolute ethanol washing for several times, dry, obtain pretreatment glass-carbon electrode；
(2) preparation of In Glassy Carbon Electrode Modified With Nano-gold: pretreatment glass-carbon electrode is put in 0.25mol/L aqueous solution of chloraurate, 4h is soaked under room temperature, with deionized water wash after taking-up, place into immersion 2h in the sodium citrate solution that mass percentage concentration is 20%, with deionized water wash after taking-up, natural drying, obtains In Glassy Carbon Electrode Modified With Nano-gold；
(3) preparation of altretamine molecularly imprinted polymer: in the reactor, be separately added into, ethanol: 42mL, Colophonium: 3g, maleic anhydride: 3g, ethylene glycol diacrylate: 6mL, chloropropene: 4.2mL, azo-bis-iso-dimethyl: 0.25g, altretamine: 0.75g, stirring and dissolving, logical noble gas deoxygenation 5min, atmosphere of inert gases, temperature rises to 75 ± 2 DEG C of stirring reaction 12h, obtains altretamine molecularly imprinted polymer colloidal sol；
(4) preparation method of altretamine molecular imprinting electrochemical sensor: take altretamine molecularly imprinted polymer colloidal sol 4 μ L and be added drop-wise on In Glassy Carbon Electrode Modified With Nano-gold, it is placed under infrared lamp, volatilize after dry solvent, used the mixed solution immersion 6h of ethanol and hydrochloric acid, remove the template molecule on electrode, with deionized water wash, natural drying, obtain altretamine molecular imprinting electrochemical sensor.
Embodiment 3
(1) pretreatment of glassy carbon electrode: by the Cr of glass-carbon electrode 0.01 ~ 0.05 μm2O3Powder carries out surface finish, then redistilled water ultrasonic cleaning is used, again with absolute ethanol washing for several times, drying up with nitrogen, be immersed in by electrode containing in the ethanol solution of the methacryloyloxypropyl methyl diethoxy silane that mass percentage concentration is 40%, temperature rises to 60 ± 2 DEG C and soaks 100min, after taking-up, with absolute ethanol washing for several times, dry, obtain pretreatment glass-carbon electrode；
(2) preparation of In Glassy Carbon Electrode Modified With Nano-gold: pretreatment glass-carbon electrode is put in 0.25mol/L aqueous solution of chloraurate, 6h is soaked under room temperature, with deionized water wash after taking-up, place into immersion 2h in the sodium citrate solution that mass percentage concentration is 25%, with deionized water wash after taking-up, natural drying, obtains In Glassy Carbon Electrode Modified With Nano-gold；
(3) preparation of altretamine molecularly imprinted polymer: in the reactor, be separately added into, ethanol: 36mL, Colophonium: 5g, maleic anhydride: 5g, ethylene glycol diacrylate: 4mL, chloropropene: 6.5mL, azo-bis-iso-dimethyl: 0.75g, altretamine: 1.5g, stirring and dissolving, logical noble gas deoxygenation 5min, atmosphere of inert gases, temperature rises to 75 ± 2 DEG C of stirring reaction 12h, obtains altretamine molecularly imprinted polymer colloidal sol；
(4) preparation method of altretamine molecular imprinting electrochemical sensor: take altretamine molecularly imprinted polymer colloidal sol 6 μ L and be added drop-wise on In Glassy Carbon Electrode Modified With Nano-gold, it is placed under infrared lamp, volatilize after dry solvent, used the mixed solution immersion 8h of ethanol and hydrochloric acid, remove the template molecule on electrode, with deionized water wash, natural drying, obtain altretamine molecular imprinting electrochemical sensor.
Embodiment 4
(1) pretreatment of glassy carbon electrode: by the Cr of glass-carbon electrode 0.01 ~ 0.05 μm2O3Powder carries out surface finish, then redistilled water ultrasonic cleaning is used, again with absolute ethanol washing for several times, drying up with nitrogen, be immersed in by electrode containing in the ethanol solution of the methacryloyloxypropyl methyl diethoxy silane that mass percentage concentration is 36%, temperature rises to 60 ± 2 DEG C and soaks 110min, after taking-up, with absolute ethanol washing for several times, dry, obtain pretreatment glass-carbon electrode；
(2) preparation of In Glassy Carbon Electrode Modified With Nano-gold: pretreatment glass-carbon electrode is put in 0.25mol/L aqueous solution of chloraurate, 4.5h is soaked under room temperature, with deionized water wash after taking-up, place into immersion 2h in the sodium citrate solution that mass percentage concentration is 24%, with deionized water wash after taking-up, natural drying, obtains In Glassy Carbon Electrode Modified With Nano-gold；
(3) preparation of altretamine molecularly imprinted polymer: in the reactor, be separately added into, ethanol: 74mL, Colophonium: 5g, maleic anhydride: 5g, ethylene glycol diacrylate: 13.3mL, chloropropene: 15mL, azo-bis-iso-dimethyl: 2.0g, altretamine: 2.0g, stirring and dissolving, logical noble gas deoxygenation 5min, atmosphere of inert gases, temperature rises to 75 ± 2 DEG C of stirring reaction 10.5h, obtains altretamine molecularly imprinted polymer colloidal sol；
(4) preparation method of altretamine molecular imprinting electrochemical sensor: take altretamine molecularly imprinted polymer colloidal sol 5 μ L and be added drop-wise on In Glassy Carbon Electrode Modified With Nano-gold, it is placed under infrared lamp, volatilize after dry solvent, used the mixed solution immersion 6.5h of ethanol and hydrochloric acid, remove the template molecule on electrode, with deionized water wash, natural drying, obtain altretamine molecular imprinting electrochemical sensor.
Embodiment 5
(1) pretreatment of glassy carbon electrode: by the Cr of glass-carbon electrode 0.01 ~ 0.05 μm2O3Powder carries out surface finish, then redistilled water ultrasonic cleaning is used, again with absolute ethanol washing for several times, drying up with nitrogen, be immersed in by electrode containing in the ethanol solution of the methacryloyloxypropyl methyl diethoxy silane that mass percentage concentration is 39%, temperature rises to 60 ± 2 DEG C and soaks 110min, after taking-up, with absolute ethanol washing for several times, dry, obtain pretreatment glass-carbon electrode；
(2) preparation of In Glassy Carbon Electrode Modified With Nano-gold: pretreatment glass-carbon electrode is put in 0.25mol/L aqueous solution of chloraurate, 5.5h is soaked under room temperature, with deionized water wash after taking-up, place into immersion 2h in the sodium citrate solution that mass percentage concentration is 23%, with deionized water wash after taking-up, natural drying, obtains In Glassy Carbon Electrode Modified With Nano-gold；
(3) preparation of altretamine molecularly imprinted polymer: in the reactor, be separately added into, ethanol: 42mL, Colophonium: 3.5g, maleic anhydride: 3.5g, ethylene glycol diacrylate: 5.2mL, chloropropene: 4.7mL, azo-bis-iso-dimethyl: 0.75g, altretamine: 0.75g, stirring and dissolving, logical noble gas deoxygenation 5min, atmosphere of inert gases, temperature rises to 75 ± 2 DEG C of stirring reaction 11.5h, obtains altretamine molecularly imprinted polymer colloidal sol；
(4) preparation method of altretamine molecular imprinting electrochemical sensor: take altretamine molecularly imprinted polymer colloidal sol 6 μ L and be added drop-wise on In Glassy Carbon Electrode Modified With Nano-gold, it is placed under infrared lamp, volatilize after dry solvent, used the mixed solution immersion 7.5h of ethanol and hydrochloric acid, remove the template molecule on electrode, with deionized water wash, natural drying, obtain altretamine molecular imprinting electrochemical sensor.
Embodiment 6
By the altretamine molecular imprinting electrochemical sensor prepared by above-described embodiment 1 ~ 5, for the detection of altretamine, step is as follows:
(1) standard solution preparation: preparing one group of altretamine (being dissolved in ethanol) standard solution including the variable concentrations of blank standard specimen, end liquid is the phosphate buffered solution of pH6.8；
(2) working curve is drawn: be reference electrode by Ag/AgCl, and platinum electrode is auxiliary electrode, of the present inventionOneThe altretamine molecular imprinting electrochemical sensor prepared by preparation method planting altretamine molecular imprinting electrochemical sensor is working electrode composition three-electrode system, connects CHI660B electrochemical workstation, at K3[Fe(CN)6] in solution, adopt cyclic voltammetry to detect in-0.10 ~ 0.9V potential range, the response current of blank standard specimen is designated asI 0 , the response current of the altretamine standard solution containing variable concentrations isI i , the difference that response current reduces is△I=I 0 -I i ,△IMass concentration with altretamine standard solutioncBetween linear, draw△I~cWorking curve；
(3) detection of altretamine: replace the altretamine standard solution in step (1) with testing sample, detects according to the method for step (2), according to the difference that response current reduces△IAnd working curve, obtain the content of altretamine in testing sample；
Described K3[Fe(CN)6] concentration of solution is 4.0mmol/L；
The concentration of the phosphate buffered solution of described pH6.8 is at 80mmol/L.
The concentration of response current and altretamine is 1.2 × 10-8~8.0×10-5In good linear relationship within the scope of mol/L, detection is limited to 1.06 × 10-8The altretamine molecular imprinting electrochemical sensor that the present invention is prepared by mol/L is used successfully in medicine, biological sample in the detection of altretamine, the response rate is between 96.26 ~ 104.32%, and the molecular engram sensor that therefore prepared by the present invention can be widely applied to the association area such as chemical industry, biological medicine detection.
Claims (6)
1.OneThe preparation method planting altretamine molecular imprinting electrochemical sensor, it is characterised in that the method has following processing step:
(1) pretreatment of glassy carbon electrode: by the Cr of glass-carbon electrode 0.01 ~ 0.05 μm2O3Powder carries out surface finish, then redistilled water ultrasonic cleaning is used, again with absolute ethanol washing for several times, drying up with nitrogen, be immersed in by electrode containing in the ethanol solution of the methacryloyloxypropyl methyl diethoxy silane that mass percentage concentration is 35 ~ 40%, temperature rises to 60 ± 2 DEG C and soaks 100 ~ 120min, after taking-up, with absolute ethanol washing for several times, dry, obtain pretreatment glass-carbon electrode；
(2) preparation of In Glassy Carbon Electrode Modified With Nano-gold: pretreatment glass-carbon electrode is put in 0.25mol/L aqueous solution of chloraurate, 4 ~ 6h is soaked under room temperature, with deionized water wash after taking-up, place into immersion 2h in the sodium citrate solution that mass percentage concentration is 20 ~ 25%, with deionized water wash after taking-up, natural drying, obtains In Glassy Carbon Electrode Modified With Nano-gold；
(3) preparation of altretamine molecularly imprinted polymer: in the reactor, add by following composition mass percentage concentration, ethanol: 56 ~ 66%, Colophonium: 5 ~ 10%, maleic anhydride: 5 ~ 10%, ethylene glycol diacrylate: 8 ~ 14%, chloropropene: 8 ~ 14%, azo-bis-iso-dimethyl: 0.5 ~ 2.0%, altretamine: 1.5 ~ 3.0%, each constituent content sum is absolutely, stirring and dissolving, logical noble gas deoxygenation 5min, atmosphere of inert gases, temperature rises to 75 ± 2 DEG C of stirring reaction 10 ~ 12h, obtains altretamine molecularly imprinted polymer colloidal sol；
(4) preparation method of altretamine molecular imprinting electrochemical sensor: take altretamine molecularly imprinted polymer colloidal sol 4 ~ 6 μ L and be added drop-wise on In Glassy Carbon Electrode Modified With Nano-gold, it is placed under infrared lamp, volatilize after dry solvent, used the mixed solution immersion 6 ~ 8h of ethanol and hydrochloric acid, remove the template molecule on electrode, with deionized water wash, natural drying, obtain altretamine molecular imprinting electrochemical sensor.
2. according to claim 1OneThe preparation method planting altretamine molecular imprinting electrochemical sensor, it is characterised in that the atmosphere of inert gases described in step (3) is that noble gas passes into until reaction terminates always.
3. according to claim 1OneThe preparation method planting altretamine molecular imprinting electrochemical sensor, it is characterised in that the noble gas described in step (3) is neon or argon.
4. according to claim 1OneThe preparation method planting altretamine molecular imprinting electrochemical sensor, it is characterised in that the mass ratio of the Colophonium described in step (3) and maleic anhydride is 1:1.
5. according to claim 1OneThe preparation method planting altretamine molecular imprinting electrochemical sensor, it is characterised in that the volume ratio of the ethanol described in step (4) and hydrochloric acid mixed solution is 20:1.
6. according to claim 1OnePlant the altretamine molecular imprinting electrochemical sensor prepared by preparation method of altretamine molecular imprinting electrochemical sensor.
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Application publication date: 20160706 |