CN112525878B - Preparation method and application of SERS substrate with filtering function - Google Patents
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Abstract
A preparation method and application of a SERS substrate with a filtering function belong to the technical field of analytical chemistry, and comprise the following steps: step 1: preparation of HCl-SnCl 2 Mixing the solutions; step 2: contacting a solid-liquid interface on one side of filter paper with HCl-SnCl prepared in advance 2 Mixing the solutions; step 3: taking out the filter paper, sequentially washing with ultrapure water and acetone, naturally airing the filter paper, and soaking the dried filter paper in AgNO 3 Soaking in the solution for a certain time, taking out filter paper with white side and dark brown side, and flushing with ultrapure water; step 4: soaking the filter paper in AgNO 3 Adding ascorbic acid solution into the solution, soaking for a certain time, taking out, and taking out againAnd cleaning with pure water to obtain the SERS substrate with the filtering function. The SERS substrate has the advantages of high filtering speed, high sensitivity, simple preparation, low cost and the like, and is suitable for quickly separating and detecting harmful substances in food.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry, and particularly relates to a preparation method and application of a SERS substrate with a filtering function.
Background
The method for separating the substances to be detected in the food comprises liquid chromatography, gas chromatography, thin layer chromatography, solvent extraction, etc. These treatments are not only complex but also costly and time consuming. Surface Enhanced Raman Scattering (SERS) spectroscopy was found in 1974 to be a technique for detecting trace substances, which is a highly sensitive, nondestructive, simple and rapid analysis method with broad prospects in the fields of material chemistry and food safety. In SERS detection, the SERS-active substrate plays a decisive role in the detection results. The traditional solid phase carrier also has higher repeatability and sensitivity, and has proper nano structure such as glass, silicon, anodic aluminum oxide and the like. However, the whole process of manufacturing these substrates is complicated, not environment-friendly and expensive, and besides, molecules of the test object cannot be sufficiently picked up when detecting complex test objects. The low-cost flexible substrate can be more suitable for picking up and detecting substances in different environments, and is widely applied to the construction active SERS substrate. Most flexible SERS substrates today are filter paper, cotton, rubberized fabric, and the like.
Disclosure of Invention
Based on the above technical background, the present invention aims to provide a preparation method of a SERS substrate with a filtration function, by selecting a carrier material of the SERS substrate and functionalizing the surface, firstly, absorbing SnCl on one side of a filter paper by solid-liquid interface contact 2 +HCl solution, reducing one side of filter paper, and depositing AgNO by electric potential 3 The reduced small-particle nano silver seeds are deposited on the surface of one side of filter paper, and the filter paper is continuously soaked in silver nitrate and ascorbic acid solution to prepare the filter function SERS substrate with controllable silver nano particle size and density. An operating method for rapid filtration and separation and SERS detection of harmful substances in food is also presented herein. The SERS substrate has the advantages of high filtering speed, high sensitivity and preparationSimple preparation, low cost and the like, and is suitable for quickly separating and detecting harmful substances in food.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
the preparation method of the SERS substrate with the filtering function comprises the steps of preparing a flexible SERS substrate with the filtering function, providing adsorption and filtering performance by taking medium-speed qualitative filter paper as a substrate, and loading nano silver particles on the surface of one side of the medium-speed qualitative filter paper through an in-situ synthesis method to form the filter paper-silver SERS substrate with the filtering function; comprises the following preparation steps:
step 1: preparation of HCl-SnCl 2 Mixing solution:
weighing SnCl 2 Dissolving the powder, ultrapure water and HCl solution to obtain HCl-SnCl 2 Mixing the solutions;
step 2: adopting an in-situ synthesis method to contact a solid-liquid interface on one side of the filter paper with HCl-SnCl prepared in advance 2 Mixing the solutions;
step 3: taking out the filter paper, sequentially washing with ultrapure water and acetone, naturally airing the filter paper, and soaking the dried filter paper in AgNO 3 Soaking in the solution for a certain time, taking out filter paper with white side and dark brown side, and flushing with ultrapure water;
step 4: soaking the filter paper in AgNO 3 And adding an ascorbic acid solution into the solution, soaking for a certain time, taking out, and cleaning with ultrapure water again to obtain the SERS substrate with the filtering function.
Further, the concentration of the HCl solution in the step 1 is 36% -38%; configured as HCl-SnCl 2 The concentration of the mixed solution is 5-30 mM.
Further, the filter paper in the step 2 is cut into 10 mm multiplied by 15 mm in advance before synthesis, and single-sided solid-liquid contact is used for adsorbing SnCl 2 The contact time of the solution was 10 min.
Further, the filter paper in the step 3 is naturally dried and then soaked in AgNO of 20 mM 3 Soaking in the solution for 10min, taking out the filter paper with dark brown color on one side, and flushing with ultrapure water.
Further, the steps are as followsThe specific method is as follows: the filter paper at this time was again soaked in 30 mM AgNO 3 Soaking in ascorbic acid solution of 40 mM for 10min, taking out, and cleaning with ultrapure water again to obtain SERS substrate with filtering function.
The SERS substrate with the filtering function is used for rapidly separating and detecting harmful substances in food.
Further, the method for separating and detecting the harmful substances in the food comprises the following steps: and respectively taking a small amount of tomato sauce and fruit juice, respectively adding thiram with different concentrations, placing the tomato sauce and the fruit juice on the blank surface of a freshly prepared flexible SERS substrate with a filtering function, staying for a period of time, detecting the target molecule thiram which is filtered and penetrated through filter paper, and detecting by using a portable Raman spectrometer to obtain a thiram Raman signal.
Further, the method for separating and detecting the harmful substances in the food comprises the following steps: respectively taking 0.15 g tomato catsup or fruit juice beverage containing different concentrations of thiram, placing a food sample on a blank surface of a SERS substrate with a filtering function, carrying out gravity filtration for 1 min, adsorbing the thiram molecules on the surface of silver nanoparticles of the substrate, and carrying out field detection by using a portable Raman spectrometer.
The invention has the advantages and effects that:
according to the invention, the flexible filter paper SERS substrate with the filtering effect is prepared for the first time, and the silver nano particles with the SERS activity are further modified on the surface of the flexible filter paper SERS substrate, so that the single-side filter paper Ag-loaded composite material with the filtering effect is prepared. The prepared composite material with the flexible filter paper loaded with Ag is successfully applied to rapid filtration separation sensitive SERS detection of thiram in food. The substrate has the advantages of filterability and separation, low cost, extremely high density, higher sensitivity for detecting trace or trace substances and the like, and the substrate has a self-filtering function, so that the separation step is omitted, and the SERS detection time is greatly shortened.
The preparation method of the SERS substrate with the filtering function and the application of the flexible SERS substrate with the filtering function to pesticide filtering separation detection in food are provided. The novel flexible SERS substrate has important significance in combination with a portable Raman spectrometer for carrying out on-site, rapid filtration and in-situ detection on the pre-filtered and separated object to be detected.
The filter type flexible SERS substrate designed in the invention is used for detecting the thiram pesticide residue in tomato sauce and fruit juice for the first time, and the filter characteristic of filter paper is beneficial to the separation and detection of special substances. The novel self-filtering type flexible SERS substrate is used for detecting thiram pesticide residues in foods, special modification of a laser instrument is not needed, pre-filtering and separation of samples are not needed, and the novel self-filtering type flexible SERS substrate is high in sensitivity, low in cost, convenient and fast to use, simple in manufacturing process and easy to produce in batches.
Drawings
FIG. 1 is a schematic illustration of the preparation and detection process of the present invention;
FIG. 2 is a graph showing the Raman spectra of filter paper substrates at different reaction times under optimal concentration conditions in example 1; (a) The raman spectrum of the filter paper substrate is shown when the reaction time of the first step and the second step is 5 min; (b) The first step of reaction time is 10min, and the second step of reaction time is 5min, and the raman spectrum of the filter paper substrate is shown; (c) The raman spectrum of the filter paper substrate is shown when the reaction time of the first step and the second step is 10 min;
FIG. 3 shows AgNO at different concentrations in example 1 3 And a raman spectrum of the PATP probe molecule filter paper substrate of ascorbic acid; (a) AgNO 3 Concentration of 10 mM and ascorbic acid concentration of 10-50 mM, (b) AgNO 3 The concentration is 20 mM, and the concentration of the ascorbic acid is 10-50 mM; (c) AgNO 3 The concentration is 30 mM, and the concentration of the ascorbic acid is 10-50 mM; (d) AgNO 3 The concentration is 40 mM and the concentration of ascorbic acid is 10-40 mM;
FIG. 4 shows (a) Ag-seed/(b) AgNO 3 A cross-sectional view of a filter paper (f) 30 mM under the optimal concentration condition of Ag particles/(c) 30 mM at a concentration of 20 mM Ag particles/(d) 40 mM Ag particles/(e) loaded with AgNPs;
FIG. 5 is an X-ray diffraction before and after loading metal nanoparticles on filter paper;
FIG. 6 is an infrared spectrogram of filter paper before and after loading metal nanoparticle;
FIG. 7 is a SERS spectrum of a flexible SERS substrate for detecting thiram pesticide in juice;
fig. 8 is a SERS spectrum of a flexible SERS substrate for detecting thiram pesticide in tomato sauce.
Detailed Description
The invention is described in further detail below with reference to the drawings and the detailed description.
The invention relates to a preparation method of a SERS substrate with a filtering function, which comprises the steps of preparing a flexible SERS substrate with the filtering function, providing adsorption and filtering performances by taking medium-speed qualitative filter paper as a substrate, and loading nano silver particles on the surface of one side of the medium-speed qualitative filter paper through an in-situ synthesis method to form the filter paper-silver SERS substrate with the filtering function. Comprises the following preparation steps:
step 1: preparation of HCl-SnCl 2 The solution was mixed.
Weighing SnCl 2 Dissolving the powder, ultrapure water and HCl solution to obtain HCl-SnCl 2 Mixed solution
Step 2: cutting filter paper into proper size in advance by adopting an in-situ synthesis method, and contacting a solid-liquid interface on one side of the filter paper with HCl-SnCl prepared in advance 2 The solution was mixed.
Step 3: taking out the filter paper, washing with ultrapure water and acetone in sequence, and naturally airing the filter paper. Soaking the dried filter paper in AgNO 3 Soaking in the solution for a certain time, taking out filter paper with white side and dark brown side, and flushing with ultrapure water.
Step 4: soaking the filter paper in AgNO 3 And adding an ascorbic acid solution into the solution, soaking for a certain time, taking out, and cleaning with ultrapure water again to obtain the SERS substrate with the filtering function.
The force of the ultrapure water and acetone washing in the steps 1-4 is not required to be excessive.
The specific process for preparing the SERS substrate with the filtering function by the in-situ synthesis method is as follows:
step 1: preparation of HCl-SnCl 2 The solution was mixed.
About 0.09g of SnCl was weighed 2 Weighing 20 ml ultrapure water, adding 33-ul HCl solution with concentration of 36-38%, dissolving the powderSolution of HCl-SnCl prepared into 5-30 mM in hydrochloric acid aqueous solution 2 Mixed solution
Step 2: adopting an in-situ synthesis method, cutting filter paper with the size of 10 mm multiplied by 15 mm in advance, and absorbing SnCl by single-sided solid-liquid contact 2 A solution.
Step 3:10 After min, the filter paper is taken out, washed by ultrapure water and acetone in sequence, and the surface residual molecules are removed. Naturally airing the filter paper and soaking in AgNO of 20 mM 3 Soaking in the solution for 10min, taking out the filter paper with dark brown color on one side, and flushing with ultrapure water. Since Ag seeds had grown to the surface of the filter paper, the color became dark brown.
Step 4: the filter paper at this time was again soaked in 30 mM AgNO 3 Soaking in ascorbic acid solution of 40 mM for 10min, taking out, and cleaning with ultrapure water again to obtain SERS substrate with filtering function.
The application of the SERS substrate with the filtering function comprises the steps of respectively taking a small amount of tomato sauce and fruit juice, respectively adding thiram with different concentrations, placing a food sample on the blank surface of the flexible SERS substrate with the filtering function, detecting the target molecule thiram which is filtered and penetrated through filter paper after 1 min, and detecting by using a portable Raman spectrometer to obtain the thiram Raman signal with lower concentration.
The method comprises the steps of respectively taking 0.15 g tomato catsup and fruit juice beverage containing the thiram with different concentrations, placing a food sample on a blank surface of a SERS substrate with a filtering function, carrying out gravity filtration for 1 min, adsorbing the thiram molecules on the surface of silver nanoparticles of the substrate, and carrying out field detection by using a portable Raman spectrometer.
Example 1
The preparation and screening steps of the flexible SERS substrate with the filtering function are as follows:
1) The first step, the single side of the filter paper is contacted and adsorbed on SnCl 2 The +HCl solution, the contact time is 5min for the first time and 10min for the second time, the solution volume is 1.0. 1.0 ml, and when the second soaking time is fixed to 5min, the contact time is obviously stronger than the Raman peak (a) corresponding to the graph of FIG. 2. Taking out the filter paper, firstly washing the two surfaces slowly by ultrapure water, and later washing the filter paper by acetone similarly slowlyAnd then dried freely in air.
2) Second step, the filter paper is soaked in 20 mM AgNO 3 When the soaking time was 10min and the solution volume was 1.0. 1.0 ml. When the optimal condition for the first step is fixed for 10min, the Raman characteristic peak showing obvious intensity is shown in the graph (c) of FIG. 2, the filter paper is taken out, and the ultra-pure water is slowly washed.
3) Third, the filter paper is soaked in 1 ml AgNO with the concentration of 10 mM, 20 mM, 30 mM (optimal concentration) 40 mM in advance 3 To the solution, 0.5 ml ascorbic acid was then added at concentrations of 10 mM, 20 mM, 30 mM, 40 mM (optimal concentration) and 50 mM, and the soaking time was fixed at 10 min. As shown in FIG. 3 (c), the optimal condition is AgNO of 30 mM 3 Solution, ascorbic acid 40 mM, yields a flexible SERS substrate with filtration function.
The average size of the silver nano particles on the surface of the filter paper synthesized by the invention is about 100 nm. As can be seen from the figure (see FIG. 4a for a silver nanoparticle scanning electron microscope image at the time of completion of the second step; FIG. 4b for AgNO) 3 Concentration 20 mM ascorbic acid concentration 40 mM;4c is AgNO 3 30 mM ascorbic acid concentration 40 mM;4d is AgNO 3 Concentration 40 mM ascorbic acid concentration 40 mM); 4e silver nanoparticle loaded cross-section; 4f is an enlarged view of silver nanoparticles; the silver nano particles in 4c are uniform in size and large in density, and are consistent with the optimal conditions for SERS detection.
The X-ray diffraction spectrum of the filter paper before and after loading the metal nano particles is shown in FIG. 5
The infrared spectrogram of the filter paper before and after loading the metal nano particles is shown in figure 6
Example 2
Preparation of flexible SERS substrate with filtering function and detection of pesticide residue in tomato sauce:
for the flexible SERS substrate with the filtering function prepared in the example 1 to be used for detecting pesticide residues in tomato catsup, the tomato catsup is respectively added with thiram with the concentration of 1000, 100, 10, 1 and 0.1 ppm in advance, the tomato catsup with the concentration of 0.15 g is taken to be placed on the blank surface of the SERS substrate with the filtering function, gravity filtration is carried out for 1 min, the thiram is permeated with filter paper, and the filter paper is adsorbed on the surface of silver nano particles of the substrate, and the portable Raman spectrometer is used for field detection.
Detection was performed using a portable raman spectrometer with proportional enhancement of raman signal with increasing concentration of thiram. As shown in fig. 7.
For SERS detection of the sample, a portable Raman spectrometer was used, BWS465 iRman plus from Bidak, the laser wavelength of which was 785 nm and the spectral resolution of which was 5 cm -1 The beam diameter was 105 microns and a quartz glass sealed window raman probe with a fiber length of 1.5 meters was used to collect the spectral signals, which were scanned 8 times.
Example 3
Preparation of a flexible SERS substrate with a filtering function and detection of pesticide residues in fruit juice:
for the application of the flexible SERS substrate with the filtering function in pesticide residue detection of fruit juice prepared in the example 1, the fruit juice is respectively added with the thiram with the concentration of 10 ul being 100, 10, 1 and 0.1 ppm, the fruit juice with fruit grains of 0.15 g is respectively taken and placed on the blank surface of the SERS substrate with the filtering function, gravity filtration is carried out for 1 min, the thiram is permeated into filter paper, and the filter paper is adsorbed on the surface of silver nano particles of the substrate, and the portable Raman spectrometer is used for field detection. Detection was performed using a portable raman spectrometer with a proportional increase in raman signal with increasing concentration of thiram. As shown in fig. 8.
For SERS detection of the sample, a portable Raman spectrometer was used, BWS465 iRman plus from Bidak, the laser wavelength of which was 785 nm and the spectral resolution of which was 5 cm -1 The beam diameter was 105 microns and a quartz glass sealed window raman probe with a fiber length of 1.5 meters was used to collect the spectral signals, which were scanned 8 times.
In summary, the invention designs and prepares the flexible SERS substrate with the filtering function for detecting the residual quantity of thiram pesticide in special foods such as tomato catsup and fruit juice. The novel flexible SERS substrate is used for detecting the residual quantity of thiram pesticides in tomato sauce and fruit juice, has the advantages of self-filterability, high sensitivity, low cost, simple manufacturing process and easy industrial batch production, and can rapidly filter impurities to achieve the purpose of detecting target molecules.
Claims (8)
1. A preparation method of a SERS substrate with a filtering function is characterized by comprising the following steps: preparing a flexible SERS substrate with a filtering function, providing adsorption and filtering performances by taking medium-speed qualitative filter paper as a substrate, and loading nano silver particles on the surface of one side of the medium-speed qualitative filter paper by an in-situ synthesis method to form the filter paper-silver SERS substrate with the filtering function; comprises the following preparation steps:
step 1: preparation of HCl-SnCl 2 Mixing solution:
weighing SnCl 2 Dissolving the powder, ultrapure water and HCl solution to obtain HCl-SnCl 2 Mixing the solutions;
step 2: adopting an in-situ synthesis method to contact a solid-liquid interface on one side of the filter paper with HCl-SnCl prepared in advance 2 Mixing the solutions;
step 3: taking out the filter paper, sequentially washing with ultrapure water and acetone, naturally airing the filter paper, and soaking the dried filter paper in AgNO 3 Soaking in the solution for a certain time, taking out filter paper with white side and dark brown side, and flushing with ultrapure water;
step 4: soaking the filter paper in AgNO 3 And adding an ascorbic acid solution into the solution, soaking for a certain time, taking out, and cleaning with ultrapure water again to obtain the SERS substrate with the filtering function.
2. The method for preparing the SERS substrate with the filtering function according to claim 1, wherein: the concentration of the HCl solution in the step 1 is 36% -38%; configured as HCl-SnCl 2 The concentration of the mixed solution is 5-30 mM.
3. The method for preparing the SERS substrate with the filtering function according to claim 1, wherein: the filter paper in the step 2 is pre-cut into 10 mm multiplied by 15 mm before synthesis, and single-sided solid-liquid contact adsorption of SnCl 2 The contact time of the solution was 10 min.
4. The method for preparing the SERS substrate with the filtering function according to claim 1, wherein: the filter paper in the step 3 is naturally dried and then soaked in AgNO of 20 mM 3 Soaking in the solution for 10min, taking out the filter paper with dark brown color on one side, and flushing with ultrapure water.
5. The method for preparing the SERS substrate with the filtering function according to claim 1, wherein: the step 4 specifically comprises the following steps: the filter paper at this time was again soaked in 30 mM AgNO 3 Soaking in ascorbic acid solution of 40 mM for 10min, taking out, and cleaning with ultrapure water again to obtain SERS substrate with filtering function.
6. The use of a SERS substrate having a filtering function according to any one of claims 1 to 5, wherein: the SERS substrate with the filtering function is used for rapidly separating and detecting harmful substances in food.
7. The use of a SERS substrate having a filtering function according to claim 6, wherein: the method for separating and detecting the harmful substances in the food comprises the following steps: and respectively taking a small amount of tomato sauce or fruit juice, respectively adding thiram with different concentrations, placing a food sample on the blank surface of the SERS substrate with the filtering function, and detecting the substrate by using a portable Raman spectrometer after 1 minute to obtain the thiram Raman signal.
8. The use of a SERS substrate having a filtering function according to claim 7, wherein: the method for separating and detecting the harmful substances in the food comprises the following steps: respectively taking 0.15 g tomato catsup or fruit juice beverage containing different concentrations of thiram, placing a food sample on a blank surface of a SERS substrate with a filtering function, carrying out gravity filtration for 1 min, adsorbing the thiram molecules on the surface of silver nanoparticles of the substrate, and detecting by using a portable Raman spectrometer.
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