CN103012806A - Synthetic method and application of polydopamine-modified carbon nanotube composite material - Google Patents
Synthetic method and application of polydopamine-modified carbon nanotube composite material Download PDFInfo
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- CN103012806A CN103012806A CN201210576446XA CN201210576446A CN103012806A CN 103012806 A CN103012806 A CN 103012806A CN 201210576446X A CN201210576446X A CN 201210576446XA CN 201210576446 A CN201210576446 A CN 201210576446A CN 103012806 A CN103012806 A CN 103012806A
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Abstract
The invention belongs to the field of nanotechnology, and particularly relates to a synthetic method and application of a polydopamine-modified carbon nanotube composite material. The synthetic method comprises the following steps in sequence: dispersing carbon nanotubes into dopamine-containing aqueous solution; quickly adding trismetyl aminomethane buffer solution into the dopamine-containing aqueous solution in which the carbon nanotubes are uniformly dispersed under magnetically stirring; mechanically stirring for 10 hours at room temperature; washing by water; and centrifugally separating to obtain the carbon nanotube composite material of which the surface is modified by polydopamine, wherein the carbon nanotube composite material shows high dispersibility in water. The polydopamine-modified carbon nanotube composite material adopts the carbon nanotubes as the framework, and therefore, a large specific surface area is provided; the polydopamine-modified carbon nanotube composite material is excellent in environmental stability and biocompatibility and high in dispersibility in water; the synthetic method is simple and low in cost; and the polydopamine-modified carbon nanotube composite material can be used as the substrate for analyzing metabolite micromolecule under high-throughput MALDI-TOFMS (Matrix Assisted Laser Desorption Ionization Time of Flight Mass Spectrometry).
Description
Technical field
The invention belongs to advanced nano material and field of nanometer technology, be specifically related to a kind of synthetic method and utilization thereof of analyzing the carbon nano tube compound material of the micromolecular poly-Dopamine HCL modification of metabolite for high-throughput MALDI-TOF MS.
Background technology
The metabolite small molecules plays vital effect in organism, by to the micromolecular detection of metabolite, can obtain a lot of information relevant with life entity.Micromolecular detection has a lot of methods to metabolite, and wherein chromatographic process is widely used.But when analyzing owing to chromatographic process, need to derive the metabolite small molecules, increase the complicacy of sample pre-treatments.Substance assistant laser desorpted ionized mass spectrum provides a kind of high-throughput, the analytical procedure that highly sensitive, analysis speed is fast.Wherein, matrix plays dilution, dispersed sample molecule, absorbs, the transfer laser energy, makes the vital role of sample ions.Yet the organic substrate that some are traditional, such as alpha-cyano-4-hydroxycinnamic acid and 2, the 5-resorcylic acid, substrate molecule can be along with the sample molecule desorption ionization, the part of low molecular mass (＜500Da) introduce more noise, what forms a lot of matrix bunch closes the peak, causes this a part of signal to noise ratio reduction, increased the mass spectrum graph complexity, severe jamming to the mensuration of low-molecular weight compound.
In recent years, many inorganic materials such as carbon nanomaterial, are widely used in MALDI detects.Carbon nanomaterial can absorb photon energy, pass to sample molecule and make its ionization, and the noise of its inferior quality end is very low, so just can obtain better resolving power and lower detectability.
Carbon nanotube (CNT) is since 1991 are found by Iijima, because its superior physical and chemical performance is widely used in many fields.Many pieces of reports show that matrix that carbon nanotube and derivative thereof can be used as MALDI-TOF-MS is applied to the detection of biomolecules in recent years.But carbon nanotube has the hydrophobicity outer wall, and easily reunion sedimentation in solution can't Uniform Dispersion, and carbon nanotube is inhomogeneous everywhere on the target spot, causes the MALDI-MS jitter, and experimental repeatability is relatively poor, easily forms sample " focus " at the sample target.
Therefore, need a kind of synthetic method and application of new carbon nano tube compound material.
Summary of the invention
The object of the invention is to provide synthetic method and the application on high-throughput MALDI mass spectroscopy metabolite small molecules thereof of a kind of surface by the carbon nano tube compound material of poly-Dopamine HCL modification.
Content of the present invention is for providing the synthetic method of a kind of surface by the carbon nano tube compound material of poly-Dopamine HCL modification, and concrete steps are as follows:
(1) is in the 40mL Dopamine HCL aqueous solution of 1mg/mL with 10mg carbon nanotube dispersed to concentration, and it is uniformly dispersed;
(2) continuing under the condition of magnetic agitation, adding 10mL concentration is the Tutofusin tris buffered soln of 10mM fast in the product of step (1) institute, and the pH of Tutofusin tris buffered soln is 8.5;
(3) with at room temperature mechanical stirring reaction of the solution of step (2) gained 10 hours;
(4) product with step (3) gained respectively washs three times with deionized water and ethanolic soln, removes impurity and the Dopamine HCL monomer on product surface;
(5) product of step (4) gained is dry in vacuum drier, namely get desired product.
Among the present invention, a kind of surface is by the application of the carbon nano tube compound material that poly-Dopamine HCL is modified: it is that the solution of 0.1mg/mL drops on the target plate of this carbon nano tube compound material as matrix that the metabolite small molecules that will need to analyze is made into concentration, in air after the seasoning, detection processed.
Among the present invention, the application of carbon nano tube compound material on high-throughput MALDI mass spectroscopy metabolite small molecules that a kind of surface is modified by poly-Dopamine HCL.
The present invention has developed the carbon nanotube modified with poly-Dopamine HCL (PD) as the method for MALDI matrix, thereby can realize very effectively that Nonparticulating sample point sample guarantees highly sensitive and high reproducible MALDI mass spectroscopy.Beneficial effect of the present invention is: the surface that provides is simple by the synthetic method of the carbon nano tube compound material that poly-Dopamine HCL is modified, material after the processing has good biocompatibility, thermostability, high sensitive and " dissolving " property in water, can be used as matrix and carries out high throughput analysis metabolite small molecules.This material provides large specific surface area take carbon nanotube as skeleton, has outstanding environmental stability and biocompatibility, good dispersity in water.Its synthetic method is simple, cost is low, has highly sensitive, signal to noise ratio high in metabolite small molecules high-throughput maldi analysis.
Description of drawings
Fig. 1 is the electron scanning micrograph of carbon nanotube;
Fig. 2 is the electron scanning micrograph that the finishing of embodiment 1 gained gathers the carbon nano tube compound material of Dopamine HCL;
Fig. 3 is the transmission electron microscope photo of carbon nanotube;
Fig. 4 is the transmission electron microscope photo that the finishing of embodiment 1 gained gathers the carbon nano tube compound material of Dopamine HCL;
Fig. 5 is the photo explanation of carbon nanotube among the embodiment 1 (left side) and surperficial carbon nano tube compound material (right side) dispersiveness in water by gathering the Dopamine HCL modification;
Fig. 6 is with the target plate point master drawing of carbon nanotube as matrix;
Fig. 7 is that the carbon nano tube compound material modified with the poly-Dopamine HCL of gained among the embodiment 2 is as the target plate point master drawing of matrix;
Fig. 8 is for to analyze Threonine (m/z=117 [M-H] by carbon nanotube as matrix
-) mass spectrum;
Fig. 9 is that the carbon nano tube compound material of being modified by poly-Dopamine HCL among the embodiment 2 is analyzed Threonine (m/z=117 [M-H] as matrix
-) mass spectrum.
Embodiment
The following examples are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1.
Synthesizing of the carbon nano tube compound material that poly-Dopamine HCL is modified
(1) with the 10mg carbon nanotube dispersed in the 40ml aqueous solution that contains the 40mg Dopamine HCL, ultrasonic 30 minutes.
(2) under the magnetic agitation that continues, in step (1) products therefrom, add fast the Tutofusin tris buffered soln (10mM, pH 8.5) of 10ml.
(3) at room temperature continue mechanical stirring 10 hours.
(4) use deionized water and washing with alcohol product each three times, centrifugation.
(5) dry in 50 ℃ vacuum drying oven.
Fig. 1 is the electron scanning micrograph of carbon nanotube; Fig. 2 is the electron scanning micrograph that the finishing of embodiment 1 gained gathers the carbon nano tube compound material of Dopamine HCL; Fig. 3 is the transmission electron microscope photo of carbon nanotube; Fig. 4 is the transmission electron microscope photo that the finishing of embodiment 1 gained gathers the carbon nano tube compound material of Dopamine HCL; Fig. 5 is the photo explanation of carbon nanotube among the embodiment 1 (left side) and surperficial carbon nano tube compound material (right side) dispersiveness in water by gathering the Dopamine HCL modification; Can find out because the introducing of poly-Dopamine HCL, make material have good wetting ability, compare as substraturn approach with the conventional carbon nanotube, because the carbon nanotube after the polymer-derived has relatively preferably hydrophilic surface, so can " dissolving " in solvent, form more uniform dispersion system, and solid suspension liquid different from the past.
Embodiment 2: carbon nano tube compound material is used for the substance assistant laser desorpted ionized mass spectroscopy metabolite of high-throughput small molecules as matrix
(1) preparation of sample: configure respectively the carbon nanotube of 1 mg/mL and the suspension liquid of carbon nano tube compound material, solvent ratio is water: ethanol=1:1(v/v), and ultrasonic.The metabolite micromolecular compound of required detection is accurate weighing and be configured to the solution of 0.1mg/ml all.Wherein sucrose, glucose, Histidine, Threonine and methionine(Met) are dissolved in water, and stearic acid and arachidic acid solution are in the mixing solutions (volume ratio is 1:1) of water and ethanol.
(2) some target: draw respectively 1 μ L carbon nanotube and carbon nano tube compound material on MALDI target plate target, place the air natural air drying under the room temperature, produce thin hypothallus; The assay solution of getting 1 μ L drips and also at room temperature place the air natural air drying on hypothallus.
(3) carbon nanotube modified with poly-Dopamine HCL of mass spectroscopy is as the metabolite small molecules of matrix, receives wooden pipe with single carbon simultaneously and analyzes the micromolecular mass spectrum of metabolite as matrix and compare.
Fig. 6 is with the target plate point master drawing of carbon nanotube as matrix; Fig. 7 is that the carbon nano tube compound material modified with the poly-Dopamine HCL of gained among the embodiment 2 is as the target plate point master drawing of matrix; Fig. 8 is for to analyze Threonine (m/z=117 [M-H] by carbon nanotube as matrix
-) mass spectrum; Fig. 9 is that the carbon nano tube compound material of being modified by poly-Dopamine HCL among the embodiment 2 is analyzed Threonine (m/z=117 [M-H] as matrix
-) mass spectrum.Can find out because the introducing of poly-Dopamine HCL; not only avoided the reunion of solid particulate; realized the liquid point sample of Nonparticulating; than the solid suspension liquid; the carbon nanotube that coats poly-Dopamine HCL is dispersed sample and make it be dispersed in uniformly in the matrix better; improve the circulation ratio of sample mass signal, and more lasting sample excitation time and the ion signal intensity of homogeneous more can be provided, be conducive to mass spectral:mass spectrographic quantitative analysis.
Claims (4)
1. the synthetic method of the carbon nano tube compound material modified by poly-Dopamine HCL of a surface is characterized in that concrete steps are as follows:
(1) is in the 40mL Dopamine HCL aqueous solution of 1mg/mL with 10mg carbon nanotube dispersed to concentration, and it is uniformly dispersed;
(2) under the condition that continues magnetic agitation, in the product of step (1) gained, add fast 10mL, pH is 8.5 Tutofusin tris buffered soln;
(3) with at room temperature mechanical stirring reaction of step (2) gained solution 10 hours;
(4) product with step (3) gained respectively washs three times with deionized water and ethanolic soln, removes impurity and the Dopamine HCL monomer on product surface;
(5) composite products of step (4) gained is dry in vacuum drier the most at last, namely gets desired product.
2. a kind of surface according to claim 1 is characterized in that by the synthetic method of the carbon nano tube compound material of poly-Dopamine HCL modification the mass ratio of carbon nanotube described in the step (1) and Dopamine HCL is 1:4.
3. the as claimed in claim 1 surface that obtains of the synthetic method application of carbon nano tube compound material in mass spectrometric detection of being modified by poly-Dopamine HCL, it is characterized in that: it is that the solution of 0.1mg/mL drops on the target plate of this carbon nano tube compound material as matrix that the metabolite small molecules that will need to analyze is made into concentration, in air, after the seasoning, carry out mass spectrometric detection.
4. application according to claim 3 is characterized in that the application of carbon nano tube compound material on high-throughput MALDI mass spectroscopy metabolite small molecules that described surface is modified by poly-Dopamine HCL.
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Application publication date: 20130403 |