CN107037102B - Nano composite material and preparation method and application thereof - Google Patents
Nano composite material and preparation method and application thereof Download PDFInfo
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- CN107037102B CN107037102B CN201710236598.8A CN201710236598A CN107037102B CN 107037102 B CN107037102 B CN 107037102B CN 201710236598 A CN201710236598 A CN 201710236598A CN 107037102 B CN107037102 B CN 107037102B
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- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
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- FYFFGSSZFBZTAH-UHFFFAOYSA-N methylaminomethanetriol Chemical compound CNC(O)(O)O FYFFGSSZFBZTAH-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
- G01N27/3278—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction involving nanosized elements, e.g. nanogaps or nanoparticles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
Abstract
The invention provides a nano composite material and a preparation method and application thereof, wherein the method comprises the following steps: the method comprises the following steps: step 1: preparing a polydopamine-modified multi-layer pore structure carbon nano material; step 2: and (3) distributing the nano metal particles on the modified material obtained in the step (1). The synthesized nano composite material can well fix lipase so as to directly detect triglyceride, and in addition, the sensor prepared by the project adopts a screen printing electrode so that the sensor has good industrial application prospect. The nano composite material can be well combined with lipase, and the screen printing electrode modified with the nano composite material on the working electrode shows good sensitivity, selectivity and anti-interference capability on the detection of triglyceride. In addition, the preparation process of the nano composite material is simple, and the screen printing electrode has the characteristics of flexibility, portability and the like; the advantages enable the triglyceride sensing chip to have great industrial application prospect.
Description
Technical Field
the invention relates to the technical field of materials, in particular to a nano composite material and a preparation method and application thereof.
Background
Triglyceride (TG) is the most abundant lipid in human body, most tissues can supply energy by using triglyceride decomposition products, and tissues such as liver and fat can synthesize triglyceride and store in fat tissue. Triglyceride levels can be classified into four grades: normal level <1.69 mM/L; the critical high level is 1.69-2.25 mM/L; the high level is 2.26 to 5.63 mM/L; the very high level is more than or equal to 5.64 mM/L. Patients with critically high and high levels of triglycerides are often associated with lipid disorders that lead to an increased risk of coronary heart disease, such as familial combined hyperlipidemia and diabetic lipid disorders. Patients with triglyceride levels above 11.3mM/L are at greatly increased risk of acute pancreatitis. Serum triglyceride elevation is a relatively common phenomenon in the elderly population, and is an important risk factor for coronary heart disease, so control of triglyceride is an important measure to reduce the onset of these diseases.
Among the various methods available for triglyceride detection, biosensors are receiving increasing attention due to their fast reaction speed, convenient operation, and high sensitivity and selectivity. However, the synthesis process of the materials of the currently reported sensor for detecting triglyceride is complicated and most of the sensors are constructed based on large electrodes such as glassy carbon electrodes, so that the sensor still in the laboratory stage cannot meet the current demand for early and rapid detection of diseases. Therefore, the synthesis of a novel nano composite material and the development of an economical and portable sensor chip capable of rapidly and accurately detecting the content of triglyceride have very important practical significance.
Disclosure of Invention
the invention aims to research a novel nano composite material with strong adsorption to lipase and application thereof, aiming at the problems of the prior complex process for manufacturing triglyceride sensor materials, poor fixation capability of the materials to lipase and the like and considering the practical significance of sensor industrialization.
a method of preparing a nanocomposite comprising the steps of:
step 1: preparing a polydopamine-modified multi-layer pore structure carbon nano material;
Step 2: distributing nano metal particles on the modified material obtained in the step (1);
Wherein, the step 2 specifically comprises the following steps:
Step (1): diluting the modified material obtained in the step 1 to obtain a solution I, and adding a certain amount of chloroauric acid into the solution I under the stirring condition, wherein the addition concentration of the chloroauric acid is 0.8-1.2 mM;
Step (2): diluting a certain amount of reducing substance with water, slowly injecting a reducing solution into the mixed solution at a speed of 0.003-0.007mL/min by using a micro-injection pump under the stirring condition, continuously stirring for 12h, and centrifugally washing for several times by using distilled water to obtain the nano metal/polydopamine/graphene nano composite material; the concentration of the reducing substance in the mixed liquid is 0.01-0.015 mol/L.
further, in the method as described above, in the step (1), the modified material obtained in the step (1) has a dilution concentration of 0.8 to 1.2 mg/mL.
further, in the method described above, the substance having reducing property in step (2) is one of sodium borohydride, formic acid, and ascorbic acid.
further, in the above method, the concentration of the reduced matter in the mixed solution in the step (2) is 0.01 to 0.015 mol/L.
Step (1): mixing the following components in a mass ratio of 1: 1, dissolving the multi-layer porous structure carbon nano material and trihydroxymethyl aminomethane in water, adjusting the pH of the solution to 8.5 by using dilute hydrochloric acid, and carrying out ultrasonic treatment for later use;
Step (2): dissolving dopamine hydrochloride with twice mass with a small amount of water, and slowly injecting the dopamine solution into the mixed solution at a certain speed under the stirring condition by using a micro-injection pump;
And (3): and after the injection is finished, continuously stirring the mixed solution for 3-4h, and then centrifugally washing the mixed solution for a plurality of times by using distilled water to remove unreacted dopamine monomers to obtain the polydopamine-modified multi-level pore structure carbon nano material.
Further, in the method as described above, the power of the ultrasonic wave in the step (1) is 60-100W.
further, the method as described above, wherein the stirring rate in the step (2) is 0.5 to 1 mL/h.
further, in the method, the carbon nanomaterial with a multi-layer pore structure is one or more of graphene, carbon nanotubes and activated carbon.
Further, in the method as described above, the nano metal particle source is one of nano gold, nano silver, nano platinum, nano palladium, nano copper and nano cobalt.
the nanocomposite obtained by the process as described in any of the above.
The application of the nano composite material prepared by the method in the aspect of preparing a sensing chip for detecting the content of triglyceride is disclosed.
has the advantages that:
the nano composite material synthesized by the invention can well fix lipase so as to directly detect triglyceride, and in addition, the sensor prepared by the project adopts a screen printing electrode so that the sensor has good industrial application prospect. The nano composite material can be well combined with lipase, and the screen printing electrode modified with the nano composite material on the working electrode shows good sensitivity, selectivity and anti-interference capability on the detection of triglyceride. In addition, the preparation process of the nano composite material is simple, and the screen printing electrode has the characteristics of flexibility, portability and the like; the advantages enable the triglyceride sensing chip to have great industrial application prospect.
drawings
FIG. 1 is a scanning electron micrograph of polydopamine/graphene oxide;
Fig. 2 is a scanning electron microscope image of nanogold/polydopamine/graphene;
FIG. 3 is a schematic diagram of the synthesis of nano-Au/poly-dopamine/graphene;
FIG. 4 is a schematic illustration of a screen printed electrode;
FIG. 5 is a graph of Cyclic Voltammetry (CV) curves at different scan rates of a fabricated triglyceride sensing chip in Phosphate Buffered Saline (PBS) containing a concentration of triglyceride;
FIG. 6 is a graph of CV oxidation peak current versus square root of scan rate for a fabricated triglyceride sensing chip in PBS containing a concentration of triglyceride;
FIG. 7 is a graph of Differential Pulse Voltammetry (DPV) response of a fabricated triglyceride sensing chip to different concentrations of triglyceride;
FIG. 8 is a graph of DPV peak current versus triglyceride concentration for different concentrations of triglyceride for the prepared triglyceride sensing chip;
fig. 9 is a bar graph of the anti-interference detection of the prepared triglyceride sensing chip.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are described below clearly and completely, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment synthesizes the nano-gold/poly-dopamine/graphene (AuNPs/PDA/RGO) nano composite material, the material can well fix lipase so as to directly detect triglyceride, and in addition, the sensor prepared by the project adopts a screen printing electrode so that the sensor has good industrial application prospect. According to the embodiment of the invention, graphene oxide is used as a carrier, and a polydopamine film is synthesized on the surface of the graphene oxide by a chemical method; and then uniformly forming long nano gold particles on the surface of the polydopamine/graphene oxide. The nanogold/polydopamine/graphene nanocomposite can be well combined with lipase, and the screen printing electrode modified with lipase/nanogold/polydopamine/graphene on the working electrode shows good sensitivity, selectivity and anti-interference capability on the detection of triglyceride. In addition, the preparation process of the nano composite material is simple, and the screen printing electrode has the characteristics of flexibility, portability and the like; the advantages enable the triglyceride sensing chip to have great industrial application prospect.
1. the preparation method of the nano composite material comprises the following steps:
(1) Preparing graphene oxide:
firstly, a certain amount of graphite powder, sodium nitrate and concentrated sulfuric acid are fully mixed under the ultrasonic condition, and then stirred in an ice bath for a period of time. Slowly adding a certain amount of potassium permanganate into the mixed solution under the condition of stirring, wherein the temperature of the mixed solution cannot be increased rapidly in the mixing process. Removing the ice bath, continuously stirring for 12 hours at normal temperature, slowly adding a certain amount of distilled water into the mixed solution, and ensuring that the temperature of the mixed solution cannot be rapidly increased in the dropping process. After the dropwise addition of the distilled water is finished, the mixed solution is firstly placed in a water bath at the temperature of 50-60 ℃ for heat preservation for 12 hours and then is placed in a water bath at the temperature of 30-35 ℃ for heat preservation for 12 hours, and the process needs to be kept for continuous stirring. Removing the water bath, and slowly dripping a certain amount of hydrogen peroxide into the mixed solution until the color of the solution becomes bright yellow. And stirring for 3 hours, and centrifugally washing the mixed solution for a plurality of times by using dilute hydrochloric acid and distilled water to obtain colloidal graphene oxide.
(2) Preparing polydopamine/graphene oxide:
The mass ratio of 1: dissolving the graphene oxide of 1 and tris (hydroxymethyl) aminomethane with water, adjusting the pH of the solution to 8.5 with dilute hydrochloric acid, and carrying out ultrasonic treatment with the ultrasonic power of 60-100W for later use. Dissolving dopamine hydrochloride with twice mass by using a small amount of water, and slowly injecting the dopamine solution into the mixed solution at the speed of 0.5-1mL/h by using a micro-injection pump under the stirring condition. And thirdly, after the injection is finished, continuously stirring the mixed solution for 3-4 hours, and then centrifugally washing the mixed solution for a plurality of times by using distilled water to remove unreacted dopamine monomers to obtain the poly-dopamine-modified graphene oxide. The morphology of the prepared polydopamine/graphene oxide can be seen in fig. 1.
(3) Preparing nano gold/polydopamine/graphene:
Prepared polydopamine/graphene oxide is diluted to the concentration of 1.0mg/mL, and a certain amount of chloroauric acid is added into the solution under the stirring condition, wherein the adding concentration is 1.0 mM. And secondly, diluting sodium borohydride with water, slowly injecting the diluted sodium borohydride into the mixed solution at a speed of 0.003-0.007mL/min by using a micro-injection pump under the stirring condition (the reduction process needs to be carried out slowly, and the nano-gold particles are aggregated due to too high stirring speed, so that the catalytic performance is poor), wherein the final concentration of the sodium borohydride in the mixed solution is 0.012mol/L, continuously stirring for 12h, and centrifugally washing for several times by using distilled water to obtain the nano-gold/polydopamine/graphene nano-composite material. Fig. 2 is an FESEM topography characterization of the prepared nano-gold/poly-dopamine/graphene, and it can be seen from fig. 2 that nano-gold particles with uniform size are well distributed on the surface of the poly-dopamine/graphene. FIG. 3 is a schematic diagram of the nanocomposite preparation process.
Wherein the dilution concentration of the polydopamine/graphene oxide can be controlled to be 0.8-1.2 mg/mL; the chloroauric acid is added at a concentration of 0.8-1.2mM (the amount of long nanogold outside this range will affect the catalytic performance by being too small or too large); the sodium borohydride can also be replaced by reducing substances such as formic acid or ascorbic acid, and the final concentration range of the reducing substances in the mixed liquid after the addition is 0.01-0.015 mol/L.
2. Preparation method of triglyceride sensing chip
(1) Taking a certain amount of nano-gold/polydopamine/graphene, preparing the nano-gold/polydopamine/graphene into a solution with the concentration of 5-10mg/mL (the solution is 50mM PBS, lipase with a certain concentration is added into the solution, and in order not to influence the activity of the enzyme, a buffer solution with neutral pH is selected for preparation, the enzyme adsorbed at a low concentration affects the detection effect less, and the electrochemical signal transmission is affected at a high concentration); (2) and (2) mixing lipase with the nano-gold/polydopamine modified graphene solution (the concentration of the lipase in the mixed solution is 5-20mg/mL), dropwise adding the mixed solution with a certain volume onto a working electrode of a screen printing electrode, airing at room temperature, and airing to obtain the triglyceride sensor. A schematic diagram of a screen printed electrode is shown in figure 4.
3. Electrochemical performance study of triglyceride sensing chip
(1) measurement of different sweep rates of the sensor chip in a PBS solution containing triglyceride. From FIGS. 5 and 6, it can be seen that the oxidation peak current and the square root of the scan rate (v) of the response of the sensor chip to triglyceride1/2) The linear relationship indicates that the reaction process of the triglyceride at the electrode surface is diffusion-controlled.
(2) The sensor chip responds to DPV of triglycerides at different concentrations. During detection, triglyceride standard solution with a certain concentration is added into PBS solution every time for DPV determination. Fig. 7 is a graph of DPV response for different concentrations of triglyceride, and fig. 8 is a graph of DPV oxidation peak current versus triglyceride concentration for different concentrations of triglyceride. From the graph, it can be seen that there is a good linear relationship between the oxidation peak current change value and the concentration of triglyceride on the prepared sensor chip.
(3) and measuring the anti-interference capability of the sensing chip. In the application, a chronoamperometry (i-t) is adopted to detect the selectivity of the lipase/nanogold/polydopamine/graphene modified screen printing electrode on triglyceride, and the interferents selected for research are substances which often coexist with the triglyceride in an actual sample, such as: uric Acid (UA), Urea (Urea), Glucose (Glucose), Cholesterol (cholestrol), and the like. As is apparent from fig. 9, when a certain concentration of triglyceride is present separately from other interfering substances, the response of the sensor chip to triglyceride is hardly affected by the other interfering substances. This shows that the sensor chip has good selectivity to triglyceride and strong anti-interference ability.
in conclusion, the nanogold/polydopamine/graphene nanocomposite can be obtained by the preparation method, the material can be well combined with lipase and has a good catalytic effect on triglyceride, and compared with a traditional sensor, the triglyceride sensing chip prepared from the nanocomposite is simpler, more economical and portable, and has a good industrial prospect. The nano gold can be nano particles of other metal elements, such as nano silver, nano platinum, nano palladium, nano copper, nano cobalt and the like, wherein the nano silver, the nano platinum, the nano palladium, the nano copper and the nano cobalt can be prepared by silver nitrate, chloroplatinic acid, chloropalladic acid, copper sulfate and cobalt chloride (cobalt nitrate) respectively; the graphene can also be one or a mixture of several of carbon nanotubes, activated carbon and a multi-layer pore structure carbon nano material.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. A method for preparing a nanocomposite, comprising the steps of:
step 1: preparing oxidized graphene modified by polydopamine;
Step 2: distributing nano metal particles on the modified material obtained in the step (1);
wherein, the step 2 specifically comprises the following steps:
Step (1): diluting the modified material obtained in the step 1 to obtain a solution I, and adding a certain amount of chloroauric acid into the solution I under the stirring condition, wherein the addition concentration of the chloroauric acid is 0.8-1.2 mM;
Step (2): diluting a certain amount of reducing substance with water, slowly injecting a reducing solution into the mixed solution at a speed of 0.003-0.007mL/min by using a micro-injection pump under the stirring condition, continuously stirring for 12h, and centrifugally washing for several times by using distilled water to obtain the nano-gold/polydopamine/graphene nano-composite material; the concentration of the reducing substance in the mixed solution is 0.01-0.015 mol/L;
The step 1 specifically comprises the following steps:
Step (a): mixing the following components in a mass ratio of 1: dissolving the graphene oxide and the tris (hydroxymethyl) aminomethane of 1 in water, adjusting the pH of the solution to 8.5 by using dilute hydrochloric acid, and carrying out ultrasonic treatment for later use;
Step (b): dissolving dopamine hydrochloride with twice mass with a small amount of water, and slowly injecting the dopamine solution into the mixed solution at a certain speed under the stirring condition by using a micro-injection pump;
Step (c): and after the injection is finished, continuously stirring the mixed solution for 3-4h, and then centrifugally washing the mixed solution for a plurality of times by using distilled water to remove unreacted dopamine monomers to obtain the polydopamine-modified multi-layer porous structure carbon nano material composite material.
2. The method according to claim 1, wherein in the step (1), the modified material obtained in the step 1 is diluted to a concentration of 0.8-1.2 mg/mL.
3. The method according to claim 1, wherein the substance having reducing property in step (2) is one of sodium borohydride, formic acid, or ascorbic acid.
4. the method of claim 1, wherein the power of the ultrasonic waves in step (a) is 60-100W.
5. The method of claim 1, wherein the injection rate in step (b) is 0.5-1 mL/h.
6. a nanocomposite prepared according to the method of any one of claims 1 to 5.
7. the use of the nanocomposite prepared according to any one of claims 1 to 5 for the preparation of a sensor chip for detecting triglyceride content;
The preparation method of the triglyceride content sensor chip comprises the following steps:
taking a certain amount of nano gold/polydopamine/graphene, and preparing the nano gold/polydopamine/graphene into a solution with the concentration of 5-10 mg/mL;
and (2) mixing lipase with the nano-gold/polydopamine modified graphene solution, dropwise adding the mixed solution with a certain volume onto a working electrode of a screen printing electrode, airing at room temperature, and airing to obtain the triglyceride sensing chip.
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