CN115060775B - Preparation of MXene-loaded gold nanocluster composite material and application of composite material as homocysteine electrochemical sensor - Google Patents
Preparation of MXene-loaded gold nanocluster composite material and application of composite material as homocysteine electrochemical sensor Download PDFInfo
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Abstract
The invention provides a preparation method of an MXene-loaded gold nanocluster composite material. First, bulk Ti is etched using LiF and concentrated HCl 3 AlC 2 Reacting to obtain the accordion-shaped two-dimensional nano material MXene. And then carrying out ultrasonic compounding on the prepared gold nanoclusters (BSA-AucNs) and MXene to obtain the MXene loaded gold nanocluster composite material BSA-AucNs/MXene. A homocysteine (Hcy) sensor is constructed by BSA-AucNs/MXene, when the Hcy concentration is within a certain concentration range, the response current Ip and the Hcy concentration are in a good linear relation, and the sensor has the advantages of wide detection range, low detection limit, simple detection process and high sensitivity, can accurately detect the Hcy in a solution and a cell lysate, and shows that the modified electrode has good application prospect in a biosensor.
Description
Technical Field
The invention relates to a preparation method of an MXene-loaded gold nanocluster composite material, and simultaneously relates to the preparation method which is used as an electrochemical sensor for detecting homocysteine (Hcy) in a solution and a cell lysate, belonging to the technical field of composite materials and the technical field of electrochemical detection.
Background
MXene is a newly discovered metal carbo/nitride with a two-dimensional layered structure in recent years and has a chemical formula of M n+ 1 X n T X Wherein (n=1-3), M represents an early transition metal such as Ti, zr, V, mo and the like; x represents C or N element, tx is a surface group, typically-OH, -O, -F and-Cl. Due to its lamellar structure similar to Graphene, the name MXene is obtained. The unique physicochemical properties of MXene, which are a new star rising in the field of nano materials, make MXene receive a great deal of attention in the fields of energy storage and conversion, sensors, multifunctional polymer composites and the like. However, single component materials often have difficulty meeting the requirements of high performance electrochemical sensing, and exploring MXene to support other premium materials is considered an effective means of solving this problem. Metal Nanoclusters (MNCs) are a class of nanomaterial with a size of less than 2 nm, formed by stacking 1 to 150 metal atoms. The metal nanocluster has a typical core-shell structure and is composed of a metal atom core and a ligand molecule shell. The ligand usually being provided with ammoniaSubstances having strong covalent interactions with metal atoms, such as thiol compounds, dendrimers, polymers, deoxyribonucleic acid (DNA), polypeptides, proteins, and the like, are used as the base, thiol, phosphorus group, and the like. Gold nanoclusters (AuNCs), silver nanoclusters (AgNCs), platinum nanoclusters (PtNCs), copper nanoclusters (CuNCs), and the like have been widely synthesized, and have recently been brought into remarkable results in biomedical fields such as biomarkers, biosensing, bioimaging, and tumor treatment. Therefore, the M NCs/MXene composite material combines the advantages of the two materials, and is expected to become an electrochemical sensing material with excellent performance.
Homocysteine (Hcy) is a sulfur-containing amino acid. Under normal conditions, hcy is catabolized in the liver, kidneys, with concentrations maintained at low levels. However, when the metabolic pathway is blocked, homocysteine accumulates in the cells and enters the blood circulation, causing chronic pathological damage. The homocysteine content in blood is an important index of human health, and if the homocysteine content is higher than 15 mu mol/L, hyperhomocysteinemia can be diagnosed. Homocysteinemia is one of independent risk factors such as heart disease, apoplexy, etc., and is regarded as the cause or result of diseases such as cancer, atherosclerosis, alzheimer's disease, etc. It was found to be associated with at least 50 diseases. Therefore, the Hcy detection method can accurately, rapidly and highly selectively detect the Hcy, and has important practical significance for life science research and clinical diagnosis. In recent years, researchers at home and abroad have conducted related research work, and reported some methods for detecting homocysteine, such as a radioactive enzyme method, an immunological method, a chromatographic method, a mass spectrometry method, a capillary electrophoresis method, a fluorescence analysis method, an electrochemical detection method and the like. The electrochemical method provides the possibility of directly and online detecting the biomolecules due to the characteristics of simple operation, high analysis speed and easy microminiaturization. Thus, electroanalytical techniques remain the first technique to detect the flux of electroactive oxidizing species.
Disclosure of Invention
The invention aims to provide a preparation method of an MXene-loaded gold nanocluster composite material;
the invention also relates to application of the MXene-loaded gold nanocluster composite material as an electrochemical sensor in detection solution and cell lysate.
1. Preparation of MXene-loaded gold nanocluster composite (BSA-AucNs/MXene)
The MXene loaded gold nanocluster composite material is obtained by loading gold nanoclusters on MXene. The method specifically comprises the following steps:
(1) Etching bulk Ti using LiF and concentrated HCl 3 AlC 2 Reacting to obtain accordion-shaped two-dimensional nano material MXene (Ti) 3 C 2 T X ). Specifically, ti is 3 AlC 2 Slowly adding the mixture of LiF and concentrated HCl, continuously stirring at 35-37 ℃ for 24-25 h, and centrifugally washing the obtained product with ultrapure water at 3500-3700 rpm until the pH value of the supernatant is 6-7. Re-dispersing the centrifuged product in ultrapure water, performing ultrasonic treatment on the product to obtain a dark green solution with the ultrasonic treatment of 1 to 2 h, and performing freeze drying on the solution to obtain the two-dimensional nanomaterial MXene (Ti) 3 C 2 T X ). Wherein Ti is 3 AlC 2 The mass ratio of the catalyst to LiF is 95:1-100:1.
(2) Mixing chloroauric acid solution and calf serum protein solution, stirring for 5-10 min, adding sodium hydroxide solution to adjust pH to 11-12, continuously stirring the mixed solution at 35-37 ℃ for 12-14 h, and dialyzing the solution through a dialysis membrane with the maximum molecular weight cutoff of 9000-10000D for 24-26 h to obtain gold nanoclusters (BSA-AucNs). Wherein the mass ratio of chloroauric acid to calf serum protein is 1:1-1:1.5.
(3) Adding MXene into BSA-AucNs solution, performing ultrasonic treatment for 5-6 h, centrifuging, and drying to obtain the MXene-loaded gold nanocluster composite material (BSA-AucNs/MXene). Wherein the mass ratio of BSA-AuCNs to MXene is 1:1.5-1:2.
2. Structural characterization of BSA-AucNs/MXene
FIG. 1 is a graph showing the morphology of MXene, BSA-AuCNs and BSA-AuCNs/MXene, wherein FIG. 1A is a Scanning Electron Microscope (SEM) of MXene, FIG. 1B, FIG. 1C and FIG. 1D are a Transmission Electron Microscope (TEM) of MXene, BSA-AuCNs and BSA-AuCNs/MXene, respectively, and the insets of FIG. 1C and FIG. 1DTEM images of BSA-AucNs and BSA-AucNs/MXene, respectively, are amplified. As shown in FIG. 1A, the MXene lamellar structure microstructure resembles an accordion due to Ti 3 AlC 2 The Al element in the film is etched to form a layered structure. From the TEM image of MXene of FIG. 1B, we can observe that the produced MXene is a typical nanoplatelet structure. The TEM image of FIG. 1C shows that the synthesized BSA-AucNs have good dispersibility. As shown in FIG. 1D, BSA-AucNs have been successfully loaded onto MXene nanoplatelets. As can be seen from the inset of FIG. 1D, there was no significant change in morphology after BSA-AuCNs were loaded on the MXene nanoplatelets. In view of the above experimental results, MXene-loaded gold nanocluster composites (BSA-AucNs/MXene) have been successfully prepared.
FIG. 2 is an X-ray diffraction spectrum (XRD) of MXene and BSA-AucNs/MXene. As shown in curve a, the diffraction peaks assigned to (002), (004), (006), (008) and (0010) were observed to correspond to MXene (Ti 3 C 2 T X ) Is a characteristic peak of (2). The XRD pattern of BSA-AucNs/MXene in curve b shows, in addition to the characteristic diffraction peak (002) of MXene, several other diffraction peaks corresponding to the diffraction of the (111), (200), (220) and (311) crystal planes of face-centered cubic gold, respectively, indicating that the BSA-AucNs/MXene material has been successfully prepared. More importantly, we can observe the position of the (002) diffraction peak of MXene at 8.76, corresponding to an interlayer spacing of 10.1A for MXene. However, the position of the (002) diffraction peak of BSA-AucNs/MXene shifts down to 8.38, with a corresponding interlayer spacing of 10.5A. This indicates that the re-stacking of MXene nanoplatelets after the introduction of BSA-AucNs is alleviated.
FIG. 3A is a nitrogen gettering chart (BET) of MXene and BSA-AucNs/MXene. Unlike the type III isotherm of MXene, BSA-AucNs/MXene exhibits the characteristics of type II isotherms, indicating that the material has improved porosity due to the simultaneous presence of mesopores and micropores. BET surface areas of BSA-AucNs/MXene and MXene are 26.5. 26.5 m, respectively 2 g -1 And 18.2. 18.2 m 2 g -1 。
FIG. 3B is a pore size distribution plot of MXene and BSA-AucNs/MXene. DFT aperture distribution diagram of BSA-AucNs/MXeneIndicating pore volume (0.097 cm) 3 g -1 ) Higher than MXene (0.056 cm) 3 g -1 ). BSA-AucNs/MXene exhibit a larger BET surface area and a higher pore volume than MXene, probably because BSA-AucNs may increase the interlayer spacing of MXene. This result is consistent with the analytical results of XRD.
3. Application of BSA-AucNs/MXene as electrochemical sensor
1. Preparation of BSA-AucNs/MXene modified electrode material
Dispersing the prepared MXene-loaded gold nanocluster composite material (BSA-AucNs/MXene) in water to prepare a dispersion liquid with the concentration of 2.5 mg/mL, dripping the dispersion liquid on a treated bare glassy carbon electrode, and drying at room temperature to prepare the modified electrode BSA-AucNs/MXene/GCE, wherein the thickness of the coating of the MXene-loaded gold nanocluster composite material (BSA-AucNs/MXene) is 200-800 nm.
2. Detection of Hcy by modified electrode
A three-electrode system is formed by taking a modified electrode BSA-AucNs/MXene/GCE as a working electrode, a platinum column as a counter electrode and a saturated calomel electrode as a reference electrode, and a phosphate buffer solution with the pH value of 0.2M and 7.0 is taken as an electrolyte, and scanning is carried out by a cyclic voltammetry. FIG. 4 is a cyclic voltammogram of bare electrode GCE (A), modified electrode BSA-AuCNs/MXene/GCE (B) in 0.2M PBS (pH=7.0) without (a) and with (B) 120. Mu.M Hcy, sweeping speed of 50 mV/s. As shown in fig. 4, each b curve of the two different modified electrodes has a higher current response than the corresponding a curve, which indicates that Hcy can generate electrochemical signals on both electrodes. By contrast, the electrochemical response signal of Hcy on BSA-AuCNs/MXene/GCE (curve of FIG. 4B b) is obviously higher than that of bare GCE (curve of FIG. 4A b), which proves that the MXene-loaded gold nanocluster composite material has a remarkable promotion effect on oxidation of Hcy and can detect Hcy more sensitively.
FIG. 5A is a timing chart of BSA-AucNs/MXene/GCE in 0.2M PBS (pH=7.0) containing different concentrations of Hcy, with an inset showing the corresponding Hcy concentration of 5.29×10 -9 ~ 0.608×10 -6 A timing diagram at M. We found that the current response increased with increasing Hcy concentration. FIG. 5When B is different in concentration, hcy is the response current Ip and the concentration [ Hcy ]]Is a linear relationship of the Hcy concentration of 5.29×10 -9 ~ 0.608×10 -6 M. As can be seen from the inset of FIG. 5B, when the Hcy concentration is 5.29×10 -9 ~ 0.608×10 -6 When the M is in the range, the linear regression equation is as follows: ip (μa) =0.443 [ Hcy ]] (μM) + 0.0196，R 2 =0.991, the equation applies for response currents Ip of 0.0219 μa to 0.289 μa; as can be seen from FIG. 5B, when the Hcy concentration is 0.608×10 -6 ~ 1.03×10 -4 At M, ip (μa) =0.0344 [ Hcy ]] (μM) + 0.273，R 2 =0.999, the equation applies for response currents Ip of 0.294 μa to 3.82 μa. As can be seen from the above, the linear range of Hcy detection was 5.29×10 -9 ~ 1.03×10 -4 M, limit of detection 1.76X10 -9 M。
3. Application of MXene loaded gold nanocluster composite material in electrochemical detection of Hcy in cell lysate.
H1299 (rat lung cancer cells) cells were obtained from the university of northwest student's college of life sciences. H1299 cells were cultured in DMEM medium containing 2 mM glutamine, 10% FBS and 100U/mL penicillin/streptomycin. To prepare H1299 cell lysate samples, the cell cells were collected and redispersed in physiological PBS buffer (0.1 m, ph=7.4). The cell dispersion was stored in a liquid nitrogen tank for 5 min and then put into water at 37 ℃ to be constantly shaken. And protein was removed from the above system using methanol at 4℃and then the mixture was centrifuged at 10000 rpm for 30 min. The supernatant from centrifugation was transferred to sterile tubes and diluted 10-fold with physiological PBS solution (0.1 m, ph=7.4) for subsequent electrochemical detection of Hcy in cell lysates. Electrochemical detection of Hcy in the diluted cell lysate was performed using the modified electrode BSA-AucNs/MXene/GCE, resulting in a Hcy of 2.18. Mu.M in the cell lysate. Thus, the concentration of Hcy in the stock solution of the H1299 cell lysate was calculated to be 21.8 μm.
In summary, compared with the prior art, the invention has the following advantages:
1. the Hcy sensor is constructed by using the MXene-loaded gold nanocluster composite material, and has the advantages of wide detection range, low detection limit, simple detection process and high sensitivity. In addition, the preparation process is simple, the cost is low, the operation is easy, and the preparation method can be used for a long time.
2. The modified electrode prepared by the invention has sensitive electrochemical response to Hcy, and the detection limit is as low as 1.76 multiplied by 10 -9 M, interference immunity is strong, stability is good.
3. The modified electrode prepared by the invention is used for electrochemical detection of Hcy in cell lysate, and the detection is accurate, which shows that the modified electrode has good application prospect in a biosensor.
Drawings
FIG. 1 is a graph of the morphology characterization of MXene, BSA-AucNs and BSA-AucNs/MXene, wherein FIG. 1A is a Scanning Electron Microscope (SEM) of MXene, and FIGS. 1B, 1C and 1D are Transmission Electron Microscope (TEM) of MXene, BSA-AucNs and BSA-AucNs/MXene, respectively.
FIG. 2 is an X-ray diffraction spectrum (XRD) of MXene and BSA-AucNs/MXene.
FIG. 3 is a graph of nitrogen gettering for MXene and BSA-AucNs/MXene (FIG. 3A) and its pore size distribution (FIG. 3B).
FIG. 4 is a cyclic voltammogram of a bare glassy carbon electrode (FIG. 4A) and a BSA-AuCNs/MXene modified electrode (FIG. 4B) in 0.2M PBS (pH=7.0) without (a) and with (B) 120 μM Hcy.
FIG. 5 is a timing diagram (FIG. 5A) of BSA-AucNs/MXene/GCE versus Hcy detection at different concentrations and a graph (FIG. 5B) of the linear relationship between Hcy concentration and its current response.
Detailed Description
The preparation of the MXene-loaded gold nanocluster composite of the present invention and the application of the modified electrode BSA-AucNs/MXene/GCE are further described below by way of specific examples.
Example 1 preparation of MXene Supported gold nanocluster composite (BSA-AucNs/MXene)
First, 2.0 g of Ti 3 AlC 2 Slowly add 1.98 g LiF and concentrated HCl (12M, 20 mL) mixed solution, continuously stir 24 h at 35 ℃, and centrifuge wash the product with ultra pure water at 3500 rpm untilThe pH of the supernatant was 6. Re-dispersing the centrifuged product in ultra-pure water, performing ultrasonic treatment on the ultra-pure water 1 h to obtain a dark green solution, and freeze-drying the dark green solution to obtain a two-dimensional nanomaterial MXene (Ti) 3 C 2 T X ) The method comprises the steps of carrying out a first treatment on the surface of the Subsequently, chloroauric acid solution (30 mL,10 mM) was slowly dropped into a flask containing calf serum protein solution (30 mL,50 mg/mL), vigorously stirred for 5 min, sodium hydroxide solution was added to adjust pH to 11, the mixed solution was continuously stirred at 35℃for 12 h, and the solution was dialyzed for 24 h through a dialysis membrane having a maximum molecular weight cut-off of 10000D to obtain gold nanoclusters (BSA-AucNs); finally, after adding the above-mentioned MXene into the above-mentioned BSA-AucNs solution and making ultrasonic treatment 5. 5 h, the mixed solution is centrifuged at 6000 rpm, and dried at 60 deg.C so as to obtain the invented MXene-loaded gold nanocluster composite material (BSA-AucNs/MXene).
EXAMPLE 2 preparation of modified electrode BSA-AucNs/MXene/GCE
(1) Pretreatment of a glassy carbon electrode: polishing the glassy carbon electrode into a mirror surface by using alumina suspension with the volume fraction of 0.30 mu m and 0.05 mu m in sequence, and then carrying out ultrasonic cleaning by using ethanol with the volume fraction of 95% and secondary distilled water in sequence to obtain a treated glassy carbon electrode; and then, performing cyclic voltammetry scanning (the scanning speed is 50 mV/s) in a 0.1M potassium chloride electrolyte solution containing 1.0 mM potassium ferricyanide probe molecules by using a three-electrode system with a glassy carbon electrode as a working electrode, a platinum column as a counter electrode and a saturated calomel electrode as a reference electrode, and finally taking out the electrode, washing with secondary distilled water and drying.
(2) Preparation of modified electrode BSA-AucNs/MXene/GCE: the MXene-loaded gold nanocluster composite material BSA-AucNs/MXene (0.0025 g) prepared in example 1 is dispersed in 1.0 mL water to prepare the composite material with the concentration of 2.5 mg mL -1 And the dispersion liquid is dripped on the treated bare glassy carbon electrode, and the modified electrode BSA-AucNs/MXene/GCE is prepared by drying at room temperature.
EXAMPLE 3 modification of Hcy concentration in electrode BSA-Au CNs/MXene/GCE detection solution
First, the arrangement concentrations were 1×10 respectively -8 M and 1X 10 -5 Hcy solution of M. Next, the modified electrodes BSA-AucNs are usedThe three-electrode system is composed of a working electrode, a platinum column as a counter electrode and a saturated calomel electrode as a reference electrode, wherein a phosphate buffer solution with Hcy of 0.2M and pH=7.0 is used as an electrolyte, and scanning is performed by a time-current method under the working potential of 0.85 and V. We obtained a concentration of 1X 10 -8 M and 1X 10 -5 Response current value of Hcy solution of M. Finally, substituting the response current into a linear regression equation Ip (μa) =0.443 [ Hcy ] of Ip and Hcy concentrations] (μM) + 0.0196，R 2 =0.991 and Ip (μa) =0.0344 [ Hcy ]] (μM) + 0.273，R 2 =0.999, and the Hcy concentrations in the test solutions were calculated to be 1.01X10, respectively -8 M and 1.02X10 -5 M. The experimental value of the concentration of Hcy in the solution is basically consistent with the theoretical value, and the modified electrode is proved to be capable of accurately detecting the concentration of Hcy in the solution.
EXAMPLE 4 detection of Hcy in cell lysates by modified electrode BSA-Au CNs/MXene/GCE
H1299 (rat lung cancer cells) cells were obtained from the university of northwest student's college of life sciences. Cells were cultured in DMEM medium containing 2 mM glutamine, 10% FBS and 100U/mL penicillin/streptomycin. To prepare H1299 cell lysate samples, the cell cells were collected and redispersed in physiological PBS buffer (0.1 m, ph=7.4). The cell dispersion was kept in a liquid nitrogen tank for 5 min and then put into 37 ℃ water to be constantly shaken. And protein was removed from the above system using methanol at 4 ℃ and then the mixture was centrifuged at 10000 rpm for 30 min. The supernatant from centrifugation was transferred to sterile tubes and diluted 10-fold with physiological PBS solution (0.1 m, ph=7.4) for subsequent electrochemical detection of Hcy in cell lysates. Electrochemical detection is carried out on Hcy in the diluted cell lysate by using a modified electrode BSA-AucNs/MXene/GCE, and the current response value of the modified electrode in the H1299 cell lysate is 0.348 mu A. Substituting the current value into equation Ip (μa) =0.0344 [ Hcy ]] (μM) + 0.273，R 2 =0.999 (this equation is applicable to response currents Ip of 0.294 μa to 3.82 μa), and the Hcy concentration in the diluted cell lysate is calculated to be 2.18 μΜ. Therefore, the concentration of Hcy in the stock solution of the H1299 cell lysate is calculated21.8. Mu.M.
Claims (5)
1. An application of an MXene-loaded gold nanocluster composite material as an electrochemical sensor in detection of homocysteine, which is characterized in that: dispersing the MXene-loaded gold nanocluster composite material in water to prepare a dispersion liquid with the concentration of 2.5 mg/mL, dripping the dispersion liquid on the treated bare glassy carbon electrode, and drying at room temperature to prepare a modified electrode BSA-AucNs/MXene/GCE; a three-electrode system is formed by taking a modified electrode BSA-AucNs/MXene/GCE as a working electrode, a platinum column as a counter electrode and a saturated calomel electrode as a reference electrode, phosphate buffer solution with the pH value of 0.2M and 7.0 is taken as electrolyte, and homocysteine with different concentrations is scanned by a time-current method under the working potential of 0.85 and V; when homocysteine concentration is 5.29×10 -9 ~ 1.03×10 -4 When the M is in the range, the response current Ip and the concentration of homocysteine have good linear relation;
the preparation method of the MXene-loaded gold nanocluster composite material comprises the following steps:
(1) Ti is mixed with 3 AlC 2 Adding LiF and concentrated HCl mixed solution, continuously stirring at 35-37 ℃ for 24-25 h, centrifugally washing the obtained product until the pH value of the supernatant is 6-7, re-dispersing the centrifuged product in ultrapure water, ultrasonically treating 1-2 h to obtain a dark green solution, and freeze-drying to obtain a two-dimensional nanomaterial MXene;
(2) Mixing chloroauric acid solution and calf serum protein solution, stirring uniformly, adding sodium hydroxide solution to adjust pH to 11-12, continuously stirring the mixed solution at 35-37 ℃ for 12-14 h, and dialyzing the solution through a dialysis membrane with the maximum molecular weight cutoff of 9000-10000D for 24-26 h to obtain gold nanoclusters BSA-AucNs;
(3) Adding MXene into BSA-AucNs solution, performing ultrasonic treatment for 5-6 h, centrifuging, and drying to obtain the MXene-loaded gold nanocluster composite BSA-AucNs/MXene.
2. The use of the MXene-loaded gold nanocluster composite as defined in claim 1 as an electrochemical sensor for detecting Hcy in a solutionThe method is characterized by comprising the following steps: in step (1), ti 3 AlC 2 The mass ratio of the catalyst to LiF is 95:1-100:1.
3. The use of the MXene-loaded gold nanocluster composite of claim 1 as an electrochemical sensor for detecting Hcy in a solution, characterized in that: in the step (2), the mass ratio of chloroauric acid to calf serum protein is 1:1-1:1.5.
4. The use of the MXene-loaded gold nanocluster composite of claim 1 as an electrochemical sensor for detecting Hcy in a solution, characterized in that: in the step (2), the mass ratio of BSA-AucNs to MXene is 1:1.5-1:2.
5. The use of the MXene-loaded gold nanocluster composite of claim 1 as an electrochemical sensor for detecting Hcy in a solution, characterized in that: the linear regression equation for the response current Ip and homocysteine concentration is:
when the Hcy concentration is 5.29×10 -9 ~ 0.608×10 -6 At M, ip=0.443 [ Hcy ]] + 0.0196，R 2 =0.991; wherein the unit of the response current Ip is μA, and the concentration of homocysteine [ Hcy ]]Is in mu M;
when the Hcy concentration is 0.608×10 -6 ~ 1.03×10 -4 At M, ip=0.0344 [ Hcy ]] + 0.273，R 2 =0.999; wherein the unit of the response current Ip is μA, and the concentration of homocysteine [ Hcy ]]In μm.
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