CN112505118B - Electrochemical sensor for detecting glucose and preparation method thereof - Google Patents
Electrochemical sensor for detecting glucose and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of electrochemical electrode material preparation, and provides an electrochemical sensor for detecting glucose and a preparation method thereof. The method has the advantages of high sensitivity and selectivity, simpler and more convenient electrode modification process, and good stability and reproducibility. Based on the cobalt @ nickel-metal organic framework-graphene (CNMs-GR) nanocomposite, a bimetallic framework is synthesized through a simple hydrothermal reaction, and the cobalt @ nickel-metal organic framework-graphene CNMs-GR nanocomposite is prepared. The sensitivity of the electrode is improved and the electrode modification process is simpler. The electrochemical sensor is used for constructing a sensing system for detecting glucose in human serum, and the selectivity of the electrode is obviously improved. The detection limit was 0.087. mu. mol/L. Wide linear range and high sensitivity.
Description
Technical Field
The invention belongs to the technical field of electrochemical electrode material preparation, and particularly relates to an electrochemical sensor for detecting glucose and a preparation method thereof.
Background
Glucose is an essential biomolecule that the human body directly participates in metabolic activities because it produces carbon dioxide and energy (ATP) through an oxidation process. However, excessive glucose levels in the blood of a human subject can cause damage to the health of the human subject, which can lead to diabetes and other complications. Diabetes, if left uncontrolled, can compromise a person's physical condition, rendering the person disabled or even dead. It has been reported that 4.15 million people face serious problems with diabetes, while 1.93 million diabetics remain undiagnosed. To overcome the health risks stemming from diabetes, the glucose concentration in the blood of a human body needs to be checked frequently. Therefore, accurate detection of glucose concentration in human blood is of great significance in the diagnosis, treatment and management of diabetes.
To date, various methods for detecting glucose have been proposed, and although these methods exhibit certain advantages, they generally involve the disadvantages of complicated sample pretreatment, long time consumption, cumbersome operation, consumption of large amounts of organic reagents, and expensive equipment. These drawbacks greatly limit their further applications. Electrochemical methods are widely used because of their low cost, high sensitivity, good selectivity and the ease of miniaturization of small volume samples.
Disclosure of Invention
The invention aims to provide an electrochemical sensor for detecting glucose and a preparation method thereof, the electrochemical sensor is prepared by modifying the surface of a glassy carbon electrode by using a nano composite material based on cobalt @ nickel-metal organic framework-graphene (CNMs-GR), and has the advantages of higher sensitivity, simpler electrode modification process, and good stability and reproducibility.
The invention is realized by the following technical scheme: an electrochemical sensor for detecting glucose is a nanocomposite material based on cobalt @ nickel-metal organic framework-graphene CNMs-GR, and the preparation method of the electrochemical sensor comprises the following steps:
(1) preparation of cobalt @ nickel-metal organic framework: adding 0.275-0.475 mmol of Co (NO)3)20.275-0.475 mmol of Ni (NO)3)2Adding 0.55 mmol-0.85 mmol of 2-amino terephthalic acid into 36 mL of solvent for 40KHz ultrasonic treatment for 30 min; reaction kettle for sealing obtained productNeutralizing and heating at 160-220 deg.c for 24 hr; naturally cooling the reaction kettle to room temperature, collecting the solid, and washing the solid with secondary water for a plurality of times; finally, the resulting solid was dried at 60 ℃ overnight to give cobalt @ nickel-metal organic framework powder; wherein: the solvent is N, N-dimethylformamide, ethanol and secondary water;
(2) preparation of cobalt @ nickel-metal organic framework-graphene CNMs-GR: adding graphene and cobalt @ nickel-metal organic framework into water to enable the concentration of the graphene to be 3.0 mg/mL-7.0 mg/mL and the concentration of the cobalt @ nickel-metal organic framework to be 5 mg/mL-10 mg/mL in a system, and carrying out ultrasonic treatment for 30min at 40KHz to form uniform dispersion liquid; vacuum drying at 60 ℃ to obtain a cobalt @ nickel-metal organic framework-graphene CNMs-GR nano composite material;
(3) preparing an electrode: dispersing 6.0 mg of cobalt @ nickel-metal organic framework-graphene CNMs-GR nano composite material in 3 mL of secondary water, and performing ultrasonic treatment for 25 min at the frequency of 40KHz to prepare a dispersion liquid with the concentration of 2.0 mg/mL; the dispersion liquid is dripped on a glassy carbon electrode, and the dripping amount is 5.0-15.0 mu L; drying for 20 min under an infrared lamp, and finally washing with secondary water to remove the loosely adsorbed composite material to obtain the cobalt @ nickel-metal organic framework-graphene CNMs-GR electrode.
Co (NO) in step (1)3)20.375 mmol; ni (NO)3)20.375 mmol; 0.75 mmol of 2-amino terephthalic acid; the solvent is a mixed solution of 32 mL of N, N-dimethylformamide, 2mL of ethanol and 2mL of secondary water; the reaction temperature in the reaction kettle was 200 ℃.
The concentration of the graphene in the step (2) is 5.0 mg/mL; the concentration of cobalt @ nickel-metal organic framework was 8.0 mg/mL; and (4) applying 10.0 mu L of the dispersion liquid drop on the surface of the glassy carbon electrode in the step (3).
The method for detecting the glucose by using the electrochemical sensor for detecting the glucose comprises the following specific steps: preparing 0.1mol of sodium hydroxide solution, and further preparing sodium hydroxide solution containing glucose; in sodium hydroxide solution containing glucose: glucose is 0.1 mmol; a three-electrode system is adopted, a cobalt @ nickel-metal organic framework-graphene CNMs-GR electrode is used as a working electrode, a silver chloride electrode is used as a reference electrode, a platinum wire is used as a counter electrode, and an electrochemical workstation is used for detecting current response to glucose concentration.
In the invention: the large surface area, excellent electrical properties, high electron mobility and high electrocatalytic activity all highlight the versatility of graphene. In addition, graphene provides abundant binding sites for non-covalent functionalization, which improves sensitivity. The amino-functionalized bimetallic organic framework has a plurality of exposed active sites and a definite pore structure, and contributes to improving the electrocatalytic capacity. The combination of Graphene (GR) and cobalt @ nickel-metal organic frameworks (CNMs) exerts a synergistic effect, contributes to the conductivity and electron transfer capability of the sensor, and improves the electrocatalytic effect on glucose.
Compared with the prior art, the invention has the advantages that: the electrode is modified on the surface of a glassy carbon electrode based on a cobalt @ nickel-metal organic framework-graphene (CNMs-GR) nanocomposite, so that the sensitivity of the electrode is improved, and the modification process of the electrode is simple. The prepared electrochemical sensor is used for constructing a sensing system for detecting glucose, and can remarkably improve the electrocatalysis of the glucose.
The electrochemical sensor prepared by the invention can detect glucose. The prepared electrochemical sensor has good stability and reproducibility, is development and application of unique properties of Graphene (GR) and cobalt @ nickel-metal organic frameworks (CNMs), and provides a new idea for future detection of glucose.
Drawings
FIG. 1 is a scanning electron microscope characterization of cobalt @ nickel-metal organic framework for preparing an electrochemical sensor according to the present invention;
FIG. 2 is a scanning electron microscope characterization image of cobalt @ nickel-metal organic framework-graphene for preparing an electrochemical sensor according to the present invention;
FIG. 3 is a cyclic voltammetry characterization of the electrode modification process for preparing an electrochemical sensor according to the present invention;
FIG. 4 is a cyclic voltammogram of glucose detected by the electrochemical sensor prepared according to the present invention;
FIG. 5 is an i-t curve of the electrochemical sensor according to the present invention with different concentrations of sodium nitrite added;
FIG. 6 is a linear relationship between glucose concentration and peak current for electrochemical sensor fabrication according to the present invention;
fig. 7 shows the stability of the cobalt @ nickel-metal organic framework-graphene electrode prepared according to the present invention to glucose detection within 15 days;
fig. 8 shows the current detection results of 6 identical cobalt @ nickel-metal organic framework-graphene electrodes prepared according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments; 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 invention relates to an electrochemical sensor prepared on the basis of a cobalt @ nickel-metal organic framework-graphene (CNMs-GR) nanocomposite material by using a glassy carbon electrode modified by the nanocomposite material, and the electrochemical sensor is used for detecting glucose in human serum. The invention is further illustrated by the following examples in conjunction with the accompanying drawings.
Example 1: an electrochemical sensor for detecting glucose is based on a cobalt @ nickel-metal organic framework-graphene (CNMs-GR) nanocomposite, and the preparation method of the electrochemical sensor comprises the following steps:
(1) preparation of cobalt @ nickel-metal organic framework: 0.375 mmol of Co (NO)3)20.375 mmol of Ni (NO)3)2And 0.75 mmol of 2-aminoterephthalic acid in 36 mL of solvent (32 mL of N.N-dimethylformamide, 2mL of ethanol and 2mL of secondary water) were sonicated. The product was sealed in a reaction kettle and heated at 200 ℃ for 24 h. The reaction kettle was then cooled to room temperature and the solid was collected and washed several times with secondary water. Finally, the resulting solid was dried at 60 ℃ overnight to give a cobalt @ nickel-metal organic framework powder.
(2) Preparation of cobalt @ nickel-metal organic framework-graphene: adding 5.0 mg/mL of graphene and 8 mg/mL of cobalt @ nickel-metal organic framework into water, and carrying out 40KHz ultrasonic treatment for 30min to form a uniform dispersion liquid. And (3) drying at 60 ℃ in vacuum to obtain the cobalt @ nickel-metal organic framework-graphene (CNMs-GR) nanocomposite.
(3) Preparing an electrode: dispersing 6.0 mg of cobalt @ nickel-metal organic framework-graphene (CNMs-GR) nano composite material in 3 mL of secondary water, and carrying out ultrasonic treatment for 25 min at the frequency of 40KHz to prepare a dispersion liquid with the concentration of 2.0 mg/mL; the dispersion liquid is dripped on a glassy carbon electrode, and the dripping amount is 10.0 mu L; drying for 20 min under an infrared lamp, and finally washing with secondary water to remove the loosely adsorbed composite material to obtain the cobalt @ nickel-metal organic framework-graphene (CNMs-GR) electrode.
And observing the prepared cobalt @ nickel-metal organic framework by using a scanning electron microscope. As shown in fig. 1, in the scanning electron microscope picture, it can be clearly seen that the cobalt @ nickel-metal organic framework is a polyhedral ball-type structure.
Scanning electron microscope characterization is carried out on the surface of the cobalt @ nickel-metal organic framework-graphene electrode prepared in example 1. As shown in fig. 2, it can be seen that the cobalt @ nickel-metal organic framework is loaded on the surface of graphene, so that the electrochemical signal of the sensor can be amplified. The success of the cobalt @ nickel-metal organic framework-graphene modified electrode prepared by the invention is demonstrated.
Example 2: an electrochemical sensor for detecting glucose is based on a cobalt @ nickel-metal organic framework-graphene (CNMs-GR) nanocomposite, and the preparation method of the electrochemical sensor comprises the following steps: 0.275 mmol of Co (NO)3)20.275 mmol of Ni (NO)3)2And 0.55 mmol of 2-aminoterephthalic acid, the graphene concentration is 3.0mg/mL, the cobalt @ nickel-metal organic framework concentration is 5mg/mL, and the amount of the dispersed liquid drop applied to the surface of the glassy carbon electrode is 5 muL. The rest of the procedure was the same as described in example 1.
Example 3: an electrochemical sensor for detecting glucose is based on a cobalt @ nickel-metal organic framework-graphene (CNMs-GR) nanocomposite, and the preparation method of the electrochemical sensor comprises the following steps: 0.475 mmol of Co (NO)3)20.475 mmol of Ni (NO)3)2And 0.85mmol 2-amino terephthalic acid is added into 36 mL solvent, the concentration of graphene is 7.0mg/mL, the concentration of cobalt @ nickel-metal organic framework is 10mg/mL, and the amount of dispersed liquid drop coated on the surface of the glassy carbon electrode is 15 muL. The rest of the procedure was the same as described in example 1.
Experimental example 1: characterization of the electrochemical sensor modification Process produced
The modified electrode prepared in example 1 was charged with 5.0 mM [ Fe (CN)6]3-/4-The solution is used as a probe to characterize the modification process of the electrode by using cyclic voltammetry. As shown in fig. 3: the peak current produced by the electrode after modification of the cobalt @ nickel-metal organic framework was slightly lower due to its poor conductivity. After Graphene (GR) is modified, the electron transfer efficiency on the surface of the electrode is accelerated, so that the peak current is obviously improved. Figure 3 illustrates that the electrode modification process prepared in example 1 was successful.
Experimental example 2: example 1 electrochemical sensor for highly sensitive detection of glucose
Taking different modified electrodes (bare electrode, cobalt @ nickel-metal organic framework-graphene) prepared in example 1, and carrying out electrochemical detection on glucose to be detected to obtain a circulating voltammogram of the glucose. After the graphene modified electrode, the current signal is obviously enhanced, and the sensitivity of the sensor is greatly improved. FIG. 4 illustrates that the electrode modification processes prepared in example 1 were successful and were able to detect glucose with high sensitivity.
Experimental example 3: detection Range of the electrochemical sensor prepared in example 1 for detecting glucose
Fig. 5 is an i-t curve of the cobalt @ nickel-metal organic framework-graphene electrode prepared according to the present invention with different concentrations of glucose added. As can be seen from FIGS. 5 and 6, in the range of 1 to 2900. mu. mol/L, the peak current of glucose is in good linear correlation with the concentration by the following equation: i ispa(μA)＝3.252+0.0369C(μmol/L)(R20.9979), detection limit was 0.087 μmol/L. This shows that the method has wide linear range and high sensitivity, and can be used for sensitively detecting glucose.
Experimental example 4: example 1 experiment of application of electrochemical sensor to detection of glucose in human serum
Standard addition methods were used for the experiments with the electrochemical sensor prepared in example 1 for the detection of glucose in human serum. As shown in Table 1, the recovery rate of the glucose sensor prepared in example 1 was 99.8% to 108% when the glucose standard solution was added to the human serum diluted 10 times, and the quantitative determination was performed using the sensor, indicating that the electrochemical sensor prepared in example 1 can be used for the determination of glucose in human serum.
Table 1 shows that the electrochemical sensor prepared by the invention is used for detecting bird glucose in human serum
Experimental example 5: stability and reproducibility verification of electrochemical sensor prepared in example 1
Fig. 7 shows the stability of the cobalt @ nickel-metal organic framework-graphene electrode prepared according to the present invention to glucose detection within 15 days. As can be seen from fig. 7, the peak current of glucose maintained good stability within 15 days. Fig. 8 shows that the peak current of glucose maintains good reproducibility for 6 identical cobalt @ nickel-metal organic framework-graphene electrodes prepared according to the present invention. The prepared electrochemical sensor has good stability and reproducibility.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (4)
1. An electrochemical sensor for detecting glucose, comprising: the electrochemical sensor for detecting glucose is a nano composite material based on cobalt @ nickel-metal organic framework-graphene CNMs-GR, and the preparation method of the electrochemical sensor comprises the following steps:
(1) preparation of cobalt @ nickel-metal organic framework: adding 0.275-0.475 mmol of Co (NO)3)20.275-0.475 mmol of Ni (NO)3)2Adding 0.55 mmol-0.85 mmol of 2-amino terephthalic acid into 36 mL of solvent for 40KHz ultrasonic treatment for 30 min; heating the product in a sealed reaction kettle at 160-220 ℃ for 24 h; naturally cooling the reaction kettle to room temperature, collecting the solid, and washing the solid with secondary water for a plurality of times; finally, the resulting solid was dried at 60 ℃ overnight to give cobalt @ nickel-metal organic framework powder; wherein: the solvent is N, N-dimethylformamide, ethanol and secondary water;
(2) preparation of cobalt @ nickel-metal organic framework-graphene CNMs-GR: adding graphene and cobalt @ nickel-metal organic framework into water to enable the concentration of the graphene to be 3.0 mg/mL-7.0 mg/mL and the concentration of the cobalt @ nickel-metal organic framework to be 5 mg/mL-10 mg/mL in a system, and carrying out ultrasonic treatment for 30min at 40KHz to form uniform dispersion liquid; vacuum drying at 60 ℃ to obtain a cobalt @ nickel-metal organic framework-graphene CNMs-GR nano composite material;
(3) preparing an electrode: dispersing 6.0 mg of cobalt @ nickel-metal organic framework-graphene CNMs-GR nano composite material in 3 mL of secondary water, and performing ultrasonic treatment for 25 min at the frequency of 40KHz to prepare a dispersion liquid with the concentration of 2.0 mg/mL; the dispersion liquid is dripped on a glassy carbon electrode, and the dripping amount is 5.0-15.0 mu L; drying for 20 min under an infrared lamp, and finally washing with secondary water to remove the loosely adsorbed composite material to obtain the cobalt @ nickel-metal organic framework-graphene CNMs-GR electrode.
2. The electrochemical sensor for detecting glucose of claim 1, wherein: co (NO) in step (1)3)20.375 mmol; ni (NO)3)20.375 mmol; 0.75 mmol of 2-amino terephthalic acid; the solvent is a mixed solution of 32 mL of N, N-dimethylformamide, 2mL of ethanol and 2mL of secondary water; the reaction temperature in the reaction kettle was 200 ℃.
3. The electrochemical sensor for detecting glucose of claim 1, wherein: the concentration of the graphene in the step (2) is 5.0 mg/mL; the concentration of cobalt @ nickel-metal organic framework was 8.0 mg/mL; and (4) applying 10.0 mu L of the dispersion liquid drop on the surface of the glassy carbon electrode in the step (3).
4. The method for detecting glucose using the electrochemical sensor for detecting glucose according to claim 1, wherein: the method comprises the following specific steps: preparing 0.1mol of sodium hydroxide solution, and further preparing sodium hydroxide solution containing glucose; 0.1mmol of glucose in sodium hydroxide solution containing glucose; a three-electrode system is adopted, a cobalt @ nickel-metal organic framework-graphene CNMs-GR electrode is used as a working electrode, a silver chloride electrode is used as a reference electrode, a platinum wire is used as a counter electrode, and an electrochemical workstation is used for detecting current response to glucose concentration.
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