CN114166818B - Hydrophobic paper surface-enhanced Raman substrate, preparation method thereof and application thereof in drug detection - Google Patents
Hydrophobic paper surface-enhanced Raman substrate, preparation method thereof and application thereof in drug detection Download PDFInfo
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Abstract
The invention belongs to the technical field of analysis and detection, and provides a high-repeatability hydrophobic paper surface enhanced Raman substrate, a preparation method thereof and application thereof in drug detection in order to solve the problems of poor stability, low repeatability and the like of the conventional paper SERS substrate; then, the paper substrate is subjected to hydrophobic treatment by OTS and MTS, and finally, the negatively charged silver nanoparticles are assembled on the surface of the paper substrate by using an ink-jet printing technology. The prepared hydrophobic paper SERS substrate greatly improves the problem of poor SERS signal detection repeatability caused by the fact that the paper base is not uniform, and the stability of the paper SERS substrate is effectively improved through the electrostatic interaction between the silver nanoparticles and the paper base. The substrate has the advantages of regular structure and low preparation cost, and can be further applied to the field detection of drug samples.
Description
Technical Field
The invention belongs to the technical field of analysis and detection, and relates to a high-repeatability hydrophobic paper surface enhanced Raman substrate, a preparation method thereof and application thereof in drug detection.
Background
In recent years, raman spectroscopy has been widely used in the fields of single molecules, environment, food safety, biosensing, biomedicine, and the like because it provides detailed information on chemical structure, crystallinity, intermolecular interaction, and the like. However, because the raman scattering area of most molecules to be measured is small, the intensity of the captured raman signal is weak, which greatly limits the application range of the raman spectroscopy technology. The Surface Enhanced Raman Spectroscopy (SERS) technology is developed on the basis of Raman Spectroscopy, and means that a noble metal material with a rough Surface is used as an SERS substrate, so that a Raman signal absorbed on a sample to be detected on the Surface of the SERS substrate can be obviously enhanced. The SERS technology effectively improves the sensitivity of the Raman detection technology and provides an analysis method with non-invasion, strong specificity and high spatial resolution.
At present, one of the most critical problems affecting the application of SERS technology is the preparation of highly repetitive, stable substrates. The filter paper is mostly applied to preparation of the paper SERS substrate in recent years due to the advantages of small fluorescence background interference, convenience in carrying, lightness, low cost and the like. In the conventional method, a hydrophobization reagent or a hydrophobic material is used to modify the surface of the sample, so that the filter paper has a hydrophobic property, and thus the sample to be detected is concentrated in a small area, a higher hot spot signal is generated, and the detection sensitivity is improved. For example, lee et al (catalytic Sensitivity of Filter Paper-Based SERS Sensor for Pesticide Detection by Hydrophobicity Change of Paper Surface [ J ]. ACS Sens, 2018, 3, 151-159.) treat Filter Paper with Alkyl Ketene Dimer (AKD), which esterify the hydroxyl groups on the Filter Paper Surface and thereby make the Filter Paper Surface somewhat hydrophobic. Compared with untreated filter paper, agNPs liquid drops dripped on the hydrophobic paper are not easy to disperse but gather in a small area, so that a higher SERS signal is generated, and the sensitivity of pesticide detection is improved. Meanwhile, researchers prepare a series of paper SERS substrates by in-situ synthesis or direct dropwise addition of noble metal nanoparticles on the surface of filter paper. For example, in 2020, godoy et al further printed a large number of gold nanorods on hydrophobic paper using inkjet printing technology to prepare highly sensitive SERS substrates (ultrasensive ink jet-printed based SERS sensor combining a high performance gold nanoparticle ink and hydrophic paper [ J ], sensors & Actuators: B. Chemical, 2020, 320, 128412).
However, since the filter paper is mainly composed of cellulose and has a large number of pores with different sizes on the surface, the nanoparticles are difficult to be uniformly distributed on the surface of the paper base, and finally the repeatability of the paper SERS substrate is poor, and the paper SERS substrate cannot be widely popularized and used. In addition, there is no interaction between the paper-based surface treated by the conventional hydrophobization method and the metal nanoparticles, resulting in difficulty in stably immobilizing the metal nanoparticles on the paper-based surface.
Disclosure of Invention
The invention provides a high-repeatability hydrophobic surface enhanced Raman substrate, a preparation method thereof and application thereof in drug detection, aiming at solving the problems of poor stability, low repeatability and the like of the conventional paper SERS substrate.
The invention is realized by the following technical scheme: a high-repeatability hydrophobic paper surface enhanced Raman substrate is characterized in that chitosan is assembled on the surface of a paper base by utilizing the electrostatic adsorption effect between the chitosan and paper base surface cellulose, so that the pores on the surface of the paper base are filled, and the surface is uniform and converted into electropositivity; then, octadecyl Trichlorosilane (OTS) and Methyl Trichlorosilane (MTS) are used for carrying out hydrophobic treatment on the paper substrate, and finally, the negatively charged silver nanoparticles are assembled on the surface of the paper substrate by using an ink-jet printing technology.
The method for preparing the high-repeatability hydrophobic paper surface enhanced Raman substrate comprises the following specific steps:
(1) Treating a paper base with chitosan: dissolving chitosan powder in acetic acid with the volume concentration of 1%, stirring for 1 hour to prepare a chitosan solution with the concentration of 3% (W/V), then uniformly coating the chitosan solution on a 3MM paper base, and drying for later use;
(2) Preparation of hydrophobizing agent: the OTS and MTS were expressed as 3:7 in the normal hexane solution, wherein the concentration of the mixed solution is 0.2 percent;
(3) Carrying out hydrophobic treatment on the paper base: placing the chitosan treated paper base obtained in the step (1) in a hydrophobization reagent for soaking for 5min, taking out, and drying at constant temperature of 40 ℃ for 5min;
(4) Uniformly printing a silver nano array: firstly, preparing silver ink used for an ink-jet printer, wherein the silver ink is prepared by centrifugally concentrating silver sol, glycerol and absolute ethyl alcohol according to a volume ratio of 65:30:10 in proportion; the preparation method comprises the following steps:
a. preparing silver sol: accurately weigh 0.0036 g of AgNO 3 Adding the powder into 198 mL of deionized water, heating in an oil bath, slightly boiling, adding 2 mL of 1% (W/V) sodium citrate solution until the color is unchanged, continuing heating for 20 min, stopping heating, and cooling to room temperature;
b. and (3) centrifugally concentrating the silver sol: 6000 Centrifuging at rpm for 10 min, discarding 95% of supernatant, and collecting silver sol precipitate;
c. obtaining of silver ink: uniformly mixing the collected silver sol precipitate with glycerol and ethanol in proportion to obtain silver ink;
d. printing a silver nano array: and (4) carrying out ink-jet printing on the hydrophobization paper base obtained in the step (3) for 12 times by using silver ink to prepare a region to be detected, and forming a reaction system, namely the high-repeatability hydrophobic paper surface enhanced Raman substrate.
The paper base is filter paper.
The drug is methamphetamine, and the specific detection method comprises the following steps: and dripping methamphetamine solutions with different concentrations into a to-be-detected area of the prepared high-repeatability hydrophobic paper surface enhanced Raman substrate, directly detecting Raman signals enhanced by molecules with different concentrations by using a Raman spectrometer, drawing a linear relation, and quantitatively detecting unknown samples.
The invention utilizes the electrostatic adsorption effect between chitosan and cellulose, and the chitosan is positively charged, so the chitosan can be assembled on the surface of the paper base through the electrostatic adsorption effect. The introduction of the chitosan effectively fills the fiber pores of the paper, so that the surface of the paper base can be smoother by filling the fiber pores of the paper, and the uniform distribution of silver nano particles is ensured. In addition, hydroxyl in chitosan molecules can further react with Octadecyl Trichlorosilane (OTS) and Methyl Trichlorosilane (MTS), so that the sensitivity of the SERS substrate is further improved, and the hydrophobic paper substrate is obtained. More importantly, the surface of the chitosan is positively charged, so that the negatively charged silver nanoparticles printed by ink-jet printing are more stably assembled on the surface of the paper base through electrostatic adsorption, and the problems of poor repeatability and stability commonly existing in the SERS paper substrate are obviously improved. The preparation method has the advantages of low cost, simple operation, excellent repeatability, stability and sensitivity.
Compared with the existing paper SERS substrate, the substrate has the unique application advantages that:
1. according to the invention, based on the electrostatic adsorption effect between chitosan and cellulose, the chitosan is used for effectively filling fiber gaps of the filter paper, the uniformity and the wrinkle resistance of the surface of the paper base are obviously improved, and a guarantee is provided for preparing the high-repeatability SERS substrate. In addition, the surface of the paper base modified by chitosan shows positive electricity, so that the negatively charged silver nanoparticles can be further fixed on the paper base through electrostatic adsorption, and the stability of the paper SERS substrate is improved.
2. The surface of the paper base modified by chitosan has a large number of hydroxyl groups, and the interaction between the hydroxyl groups and Octadecyl Trichlorosilane (OTS) and Methyl Trichlorosilane (MTS) is utilized to obtain the high-hydrophobicity paper base. The hydrophobic effect effectively shortens the gap between the metal nano particles and molecules, generates a large number of SERS hot spots, and obviously improves the detection sensitivity.
3. The uniform hydrophobic paper SERS substrate developed by the invention has the advantages of simple preparation process, low cost and combination with the advantages of ink-jet printing, can be produced in large scale, and provides a portable, high-sensitivity, high-repeatability and high-stability signal enhancement substrate for the multi-field application of the SERS technology.
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In order to describe the detection method of the present invention more clearly, the following will describe the technical solution in the embodiment of the present invention clearly and completely with reference to the drawings in the embodiment of the present invention.
FIG. 1 is an SEM image and optical micrograph of untreated, chitosan-treated, chitosan-hydrophobically treated 3MM filter paper; in the figure: (a) is SEM picture; (b) is an optical microscopy image;
FIG. 2 (a) is a photograph taken with a cell phone of silver ink printed on hydrophobic paper; (b) Printing a silver ink picture on the high-repeatability hydrophobic paper surface enhanced Raman substrate prepared by the invention, wherein the picture is shot by a mobile phone; (c) is an SEM image of the printed silver ink area in figure (b);
FIG. 3 is a 3D waterfall plot of hydrophobically treated filter paper and hydrophobic-chitosan treated filter paper; in the figure: (a) is a 3D waterfall plot of hydrophobically treated filter paper; (b) is a 3D waterfall plot of the hydrophobic-chitosan treated filter paper;
FIG. 4 is a graph of the stability of the hydrophobically treated filter paper and the hydrophobic-chitosan treated filter paper over 10 days, in which: (a) Stability of hydrophobically treated filter paper, (b) stability of hydrophobically-chitosan treated filter paper;
fig. 5 is a raman spectrogram of methamphetamine molecules with different concentrations detected on the highly-repetitive hydrophobic paper surface-enhanced raman substrate prepared by the method, wherein the final detection concentration is 0.1 ppb.
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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1: a high-repeatability hydrophobic paper surface enhanced Raman substrate is characterized in that chitosan is assembled on the surface of a paper base by utilizing the electrostatic adsorption effect between the chitosan and paper base surface cellulose, so that the pores on the surface of the paper base are filled, and the surface of the paper base is uniform and is converted into electropositivity; then, the paper substrate is subjected to hydrophobic treatment by using Octadecyl Trichlorosilane (OTS) and Methyl Trichlorosilane (MTS), and finally, the negatively charged silver nanoparticles are assembled on the surface of the paper substrate by using an ink-jet printing technology.
The preparation method comprises the following steps:
(1) Treating a paper base with chitosan: dissolving chitosan powder in acetic acid with the volume concentration of 1% to prepare chitosan solution with the concentration of 3% (W/V), then uniformly coating the chitosan solution on 3MM filter paper, and drying for later use;
(2) Preparation of hydrophobizing agent: the OTS and MTS were mixed as follows: 7 is mixed in the normal hexane solution, and the concentration of the mixed solution is 0.2 percent;
(3) Carrying out hydrophobic treatment on the paper base: placing the chitosan treated paper base obtained in the step (1) in a hydrophobization reagent for soaking for 5min, taking out, and drying in a drying oven at the constant temperature of 40 ℃ for 5min; after drying, the filter paper was removed and the contact angle of the filter paper was recorded using a contact angle meter.
SEM images and optical micrographs of untreated, chitosan-treated, chitosan-hydrophobically treated 3MM filter paper are shown in FIG. 1, from which it can be seen that the filter paper treated with chitosan has significantly reduced porosity and a smoother surface, and that further hydrophobic treatment does not affect the smoothness and structure of the filter paper surface.
(4) Uniformly printing a silver nano array: firstly, preparing silver ink used for an ink-jet printer, wherein the silver ink is prepared by centrifugally concentrating silver sol, glycerol and absolute ethyl alcohol according to a volume ratio of 65:30:10 in proportion; the preparation method comprises the following steps:
a. preparing silver sol: accurately weigh 0.0036 g of AgNO using an electronic balance 3 Adding the powder into 198 mL of deionized water, heating in an oil bath, slightly boiling, adding 2 mL of 1% (W/V) sodium citrate solution until the color is unchanged, continuing heating for 20 min, stopping heating, and cooling to room temperature;
b. and (3) centrifugally concentrating the silver sol: centrifuging at 6000 rpm for 10 min, discarding 95% of supernatant, and collecting silver sol precipitate;
c. obtaining of silver ink: and mixing the collected silver sol precipitate with glycerol and ethanol according to a volume ratio of 65:30:10, mixing uniformly to obtain silver ink;
d. printing a silver nano array: and (4) performing ink-jet printing on the hydrophobization paper base obtained in the step (3) by using silver ink for 12 times by using an ink-jet printer to prepare a region to be detected, and forming a reaction system, namely the high-repeatability hydrophobization paper surface enhanced Raman substrate.
Fig. 2 is a photograph taken by a cell phone of silver ink printed on hydrophobic paper (a) and hydrophobic-chitosan paper (b), and (c) is an SEM image of the area of the silver ink printed in fig. (b). As can be seen from the figure, the color of the silver ink printed on the hydrophobic-chitosan paper base is relatively uniform, i.e. the silver nanoparticles are distributed relatively uniformly.
The detection method of the methamphetamine specifically comprises the following steps: and dripping methamphetamine solutions with different concentrations into a to-be-detected area of the prepared high-repeatability hydrophobic paper surface enhanced Raman substrate, directly detecting Raman signals enhanced by molecules with different concentrations by using a Raman spectrometer, drawing a linear relation, and quantitatively detecting unknown samples.
FIG. 3 is a 3D waterfall plot of (a) hydrophobically treated filter paper and (b) hydrophobic-chitosan treated filter paper. From the figure, it can be seen that the hydrophobic-chitosan paper base surface is relatively uniform compared with the filter paper which is subjected to pure hydrophobic treatment. (a) (b) the relative standard deviation RSD at peak 1621 was 12.7% and 3.65%, respectively.
FIG. 4 is a graph of the stability of (a) hydrophobically treated filter paper and (b) hydrophobic-chitosan treated filter paper over 10 days. Measurement with hydrophobic paper 10 -6 Raman intensity of M CV, found a 78.1% decrease in intensity at 1621 peak after 10 days, while the intensity measured for hydrophobic-chitosan paper was essentially unchanged.
Fig. 5 is a raman spectrum of methamphetamine molecules with different concentrations detected on a hydrophobic-chitosan paper SERS substrate, and the final detection concentration is 0.1 ppb.
The experiment results show that the chitosan is used for effectively filling fiber gaps of the filter paper based on the electrostatic adsorption effect between the chitosan and the cellulose, so that the uniformity and the wrinkle resistance of the surface of the paper base are obviously improved, the surface of the paper base modified by the chitosan has positive electricity, the silver nanoparticles with negative electricity can be further fixed on the paper base through the electrostatic adsorption effect, and the stability of the SERS substrate is improved; the surface of the paper base modified by chitosan has a large number of hydroxyl groups, and the interaction between the hydroxyl groups and Octadecyl Trichlorosilane (OTS) and Methyl Trichlorosilane (MTS) is utilized to obtain the high-hydrophobicity paper base. The hydrophobic effect effectively shortens the gap between the metal nanoparticles and molecules, generates a large number of SERS hot spots, and obviously improves the detection sensitivity.
The surface of the chitosan is positively charged, so that the negatively charged silver nanoparticles for ink-jet printing are more stably assembled on the surface of the paper base through electrostatic adsorption, and the problems of poor repeatability and stability commonly existing in the SERS paper base are obviously solved. The preparation method has the advantages of low cost, simple operation, excellent repeatability, stability and sensitivity.
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 these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (4)
1. A hydrophobic paper surface enhanced Raman substrate is characterized in that: the chitosan is assembled on the surface of the paper base by utilizing the electrostatic adsorption effect between the chitosan and the cellulose on the surface of the paper base, so that the pores on the surface of the paper base are filled, and the surface is uniform and is converted into positive electricity; then, octadecyl Trichlorosilane (OTS) and Methyl Trichlorosilane (MTS) are used for carrying out hydrophobic treatment on the paper substrate, and finally, the negatively charged silver nanoparticles are assembled on the surface of the paper substrate by using an ink-jet printing technology.
2. A method of preparing a hydrophobic paper surface-enhanced raman substrate of claim 1, wherein: the method comprises the following specific steps:
(1) Treating the paper base with chitosan: dissolving chitosan powder in acetic acid with the volume concentration of 1% to prepare a chitosan solution with the concentration of 3% (W/V), then uniformly coating the chitosan solution on a 3MM paper base, and drying for later use;
(2) Preparation of hydrophobizing agent: the OTS and MTS were mixed as follows: 7 is mixed in the normal hexane solution, and the concentration of the mixed solution is 0.2 percent;
(3) Hydrophobization treatment of paper base: placing the chitosan treated paper base obtained in the step (1) in a hydrophobization reagent for soaking for 5min, taking out the paper base, and drying the paper base at the constant temperature of 40 ℃ for 5min;
(4) Uniformly printing a silver nano array: firstly, preparing silver ink for an ink-jet printer, wherein the silver ink is prepared by mixing centrifugally concentrated silver sol, glycerol and absolute ethyl alcohol in a volume ratio of 65:30:10 in proportion; the preparation method comprises the following steps:
a. preparing silver sol: accurately weigh 0.0036 g of AgNO 3 Adding the powder into 198 mL of deionized water, heating in an oil bath, slightly boiling, adding 2 mL of 1% (W/V) sodium citrate solution, waiting until the color is unchanged, continuing heating for 20 min, stopping heating, and cooling to room temperature;
b. centrifugally concentrating the silver sol: 6000 Centrifuging at rpm for 10 min, discarding 95% of supernatant, and collecting silver sol precipitate;
c. obtaining of silver ink: uniformly mixing the collected silver sol precipitate with glycerol and ethanol in proportion to obtain silver ink;
d. printing a silver nano array: and (4) performing ink-jet printing on the hydrophobic paper base obtained in the step (3) for 12 times by using silver ink to prepare a region to be detected, and forming a reaction system, namely the hydrophobic paper surface enhanced Raman substrate.
3. The method of making a hydrophobic paper surface-enhanced raman substrate of claim 2, wherein: the paper base is filter paper.
4. The use of the hydrophobic paper surface enhanced raman substrate prepared by the method of claim 2 in drug detection, wherein: the drug is methamphetamine, and the specific detection method comprises the following steps: and dripping methamphetamine solutions with different concentrations into a to-be-detected area of the prepared hydrophobic paper surface enhanced Raman substrate, directly detecting Raman signals enhanced by molecules with different concentrations by using a Raman spectrometer, drawing a linear relation, and quantitatively detecting unknown samples.
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| US10379053B2 (en) * | 2015-06-02 | 2019-08-13 | University-Industry Cooperation Group Of Kyung Hee University | Paper-based surface-enhanced raman scattering substrate, and preparation method therefor |
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