CN105606587B - Enrofloxacin detection method based on nano-Ag particles Yu carborundum paper SERS substrates - Google Patents
Enrofloxacin detection method based on nano-Ag particles Yu carborundum paper SERS substrates Download PDFInfo
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Abstract
The Enrofloxacin detection method based on nano-Ag particles Yu carborundum paper SERS substrates that the invention discloses a kind of comprising following steps：It takes silver nano-particle solution and carries out eccentric cleaning, remove supernatant, then the deposit made is suspended in ethanol solution and obtains aaerosol solution；The mixed solution that Enrofloxacin standard sample solution forms Enrofloxacin and Nano silver grain is added；Mixed solution is added drop-wise in SERS substrates again, obtains standard detection substrate；The SERS spectra of the substrate of measurement standard detection later；When detection, extracts detectable substance and dissolving forms detected sample solution, detected sample solution is mixed with aaerosol solution, then the mixed solution is added drop-wise in SERS substrates, obtains substrate to be detected, measures the SERS spectra of substrate to be detected；If two SERS spectras are identical, show to contain Enrofloxacin in substrate to be detected；Advantage is to realize based on nano-Ag particles and detection application of the carborundum paper SERS substrates to Enrofloxacin, and have very high detection sensitivity.
Description
Technical field
The present invention relates to a kind of Enrofloxacin (Enrofloxacin, C19H22FN3O3) detection technique, more particularly, to one
Kind is based on nano-Ag particles and silicon carbide (SiC) sand paper SERS (Surface-enhanced Raman scattering, surface
Enhance Raman scattering) substrate Enrofloxacin detection method.
Background technology
Since Surface enhanced Raman scattering (SERS) spectral technique has many advantages, such as highly sensitive, lossless and fingerprint spectrum signature
And it is widely used in the various fields such as analytical chemistry, environmental science and biomedicine.For SERS spectra technology, prepare
The surface topography of noble metal (such as gold, silver and copper) nano-particle and noble metal SERS substrates have for the enhancing of SERS signal
It seriously affects.Usually, noble metal nano particles and the surface of noble metal SERS substrates are more coarse, and the enhancing of SERS signal is got over
Greatly.Therefore, people are prepared for the noble metal nano particles and noble metal SERS substrates of various patterns, to obtain the Gao Ling of sample
Sensitivity SERS spectra detects.The preparation of noble metal nano particles mainly has physical method and chemical method.Physical method is prepared into
The size uniform of the noble metal nano particles arrived, size are controllable, but step is more, time-consuming, of high cost, and chemical method can be with
Inexpensive batch prepares the noble metal nano particles of different morphologies.The preparation method of noble metal SERS substrates mainly has following three
Kind：The first is that the noble metal nano particles colloidal sol for directly preparing chemical synthesis is coated in carrying template as SERS bases
Bottom；Second is that the methods of physics, chemistry or electrochemistry deposited metal nanometer is utilized in the carrying template for be carved with array pattern
Particle obtains metal nano particles array SERS substrates；The third is to utilize parents' molecule, will be golden by electrostatic or chemical method
Category self-assembly is fixed in carrying template (such as silicon chip or glass) and forms SERS substrates.Comparatively, the first
Method is relatively easy, can be mass, but the SERS signal that the SERS substrates prepared generate is weaker；Prepared by second method
Strong SERS signal can be obtained in SERS substrates, and with good stability and repeated, but complex manufacturing technology, cost compared with
It is high；The SERS substrates that the third method obtains have higher SERS signal, but stability and less reproducible deficiency.
On the other hand, Enrofloxacin is a kind of preparing fluoroquinolone compound class antibiotic, due to it with broad spectrum antibiotic activity and
Very strong permeability can effectively kill the various bacteria in animal body.Although Enrofloxacin is a kind of effective antiseptic,
But the proliferation that Enrofloxacin also results in environmental pollution, promotes antibiotic resistant bacteria in aquatic environment is excessively used, with
And the side effects such as micropopulation in change human body intestinal canal, bring grave danger to people's health.Therefore, to food and environment
In the content of Enrofloxacin be detected, be very necessary.Currently, the detection method to Enrofloxacin mainly has liquid phase color
Spectrum-tandem mass spectrometry, time resolved fluoro-immunoassay (TRFIA) technology, chemiluminescent enzyme-linked immunosorbent immune detection.These types of method
With high detection sensitivity, but testing cost is high, time loss is long, and the requirement to tester's specialized capability is high, thus
Influence the commonly used of them.
Invention content
Technical problem to be solved by the invention is to provide one kind based on nano-Ag particles and carborundum paper SERS substrates
Enrofloxacin detection method, by the enhancing of SERS signal realize to Enrofloxacin high sensitivity detection.
Technical solution is used by the present invention solves above-mentioned technical problem：One kind being based on nano-Ag particles and silicon carbide sand
The Enrofloxacin detection method of paper SERS substrates, it is characterised in that in conjunction with Nano silver grain and carborundum paper SERS substrates to grace
Flucloxacillin is detected, and is as follows：
Step 1：It takes silver nano-particle solution to inject centrifuge tube, eccentric cleaning then is carried out to silver nano-particle solution, is connect
It and removes supernatant after eccentric cleaning, retain the Nano silver grain for being deposited in centrifugation bottom of the tube, then by Nano silver grain
Deposit is suspended in the ethanol solution that mass percentage concentration is 50%, and the suspension for obtaining monodispersed homogenous silver nano particle is molten
Liquid；
Step 2：The aaerosol solution for the monodispersed homogenous silver nano particle being prepared in step 1 is taken, while will be pure
The Enrofloxacin standard sample that degree is configured to a concentration of 0.01~5 mg/litre more than or equal to 98% Enrofloxacin powder is molten
Then Enrofloxacin standard sample solution is added in the aaerosol solution of the monodispersed homogenous silver nano particle taken and mixes by liquid
The mixed solution for forming Enrofloxacin and Nano silver grain is closed, then the mixed solution of Enrofloxacin and Nano silver grain is surpassed
Sonication；
Step 3：The mixed solution for the Enrofloxacin and Nano silver grain that step 2 is prepared is taken, and is added drop-wise to carbonization
It in silica sand paper SERS substrates, then is dried at room temperature for, obtains the standard detection substrate of Enrofloxacin；
Step 4：Vertical irradiation is on the standard detection substrate of Enrofloxacin after making the laser line focus that laser emits,
The laser of irradiation is received after the standard detection substrate reflection of Enrofloxacin by Raman spectrometer, and Raman spectrometer shows grace fluorine
The SERS spectra of the standard detection substrate of Sha Xing；
Step 5：Before actually detected, detectable substance is extracted, and dissolve detectable substance and obtain detected sample solution；Then step is taken
The aaerosol solution for the monodispersed homogenous silver nano particle being prepared in rapid one；Then the detected sample solution of preparation is added
Enter into the aaerosol solution of the monodispersed homogenous silver nano particle taken to be mixed to form the mixed of Enrofloxacin and Nano silver grain
Solution is closed, then the mixed solution of Enrofloxacin and Nano silver grain is ultrasonically treated；Grace after later will be sonicated
The mixed solution of Flucloxacillin and Nano silver grain is added drop-wise in carborundum paper SERS substrates, then is dried at room temperature for, and grace is obtained
The substrate to be detected of Flucloxacillin；
Step 6：When actually detected, vertical irradiation is in the to be checked of Enrofloxacin after making the laser line focus of laser transmitting
It surveys on substrate, the laser of irradiation is received after the substrate reflection to be detected of Enrofloxacin by Raman spectrometer, and Raman spectrometer is aobvious
The SERS spectra of the substrate to be detected of Enrofloxacin is shown；Then compare Enrofloxacin standard detection substrate SERS spectra with
The SERS spectra of the substrate to be detected of Enrofloxacin, if the SERS spectra of the substrate to be detected of Enrofloxacin and Enrofloxacin
The SERS spectra of standard detection substrate is identical, then shows to contain Enrofloxacin in the substrate to be detected of Enrofloxacin, that is, show to examine
It surveys in object and contains Enrofloxacin；If the SERS spectra of the substrate to be detected of Enrofloxacin and the standard detection substrate of Enrofloxacin
SERS spectra differ, then show not contain Enrofloxacin in the substrate to be detected of Enrofloxacin, that is, show in detectable substance not
Contain Enrofloxacin.
The preparation process of silver nano-particle solution is in the step one：A1, analytically pure silver nitrate is taken at room temperature
Powder, and be dissolved in deionized water and be stirred for uniformly obtaining the silver nitrate that mass percentage concentration is 0.009%~0.018%
Solution；Then it is heated to boiling while being stirred silver nitrate solution；A2, analytically pure sodium citrate solution is added dropwise
The mass percent for entering into the silver nitrate solution of boiling, and persistently stirring to get sodium citrate be 0.03%~0.06% it is mixed
Solution is closed, until after the color of the mixed solution of boiling becomes celadon, cools down at room temperature, obtains monodispersed a diameter of 25
~80 nanometers of homogenous silver nano particle solution.
Ranging from 100~500 microlitres of institute's taken amount of silver nano-particle solution in the step one；The step one
Ranging from 25~500 microlitres of institute's taken amount of middle ethanol solution；The institute of Enrofloxacin standard sample solution in the step two
Ranging from 25~150 microlitres of taken amount；Institute's taken amount of the mixed solution of Enrofloxacin and Nano silver grain in the step three
Ranging from 25~50 microlitres.
Be 5000~11000 revs/min to the rotating speed of silver nano-particle solution progress eccentric cleaning in the step one,
Scavenging period is 5~30 minutes.
The processing time that the mixed solution of Enrofloxacin and Nano silver grain is ultrasonically treated in the step two
It is 10~30 minutes.
The preparation process of carborundum paper SERS substrates is in the step three and the step five：By regular shape
Carborundum paper be placed in rf magnetron sputtering system, and control magnetic control sputtering system operating pressure be 0.1~1.4 pa,
Sputtering power is 50~150 watts, and deposition thickness is on carborundum paperSilver, obtain with silicon carbide sand
Paper is the carborundum paper SERS substrates of template.
The mesh number of the carborundum paper is 240~5000 mesh.
The time of integration that SERS spectra is acquired in the step four and the step six is 1~10 second, irradiates laser
Power be 3~30 milliwatts, optical maser wavelength be 785 nanometers.
The aaerosol solution of detected sample solution and the monodispersed homogenous silver nano particle taken in the step five
Volume ratio be 3：2；The processing time of supersound process is 10~30 minutes；Enrofloxacin after sonicated and nano grain of silver
Institute's taken amount of the mixed solution of son is 25~50 microlitres.
Compared with the prior art, the advantages of the present invention are as follows：
1) micro highly sensitive detection can be carried out to Enrofloxacin using the method for the present invention.
2) mixed solution of Enrofloxacin and Nano silver grain is added drop-wise to carborundum paper SERS substrates by the method for the present invention
On, the SERS signal intensity of carborundum paper SERS substrates is further enhanced, detection sensitivity is improved.
3) Enrofloxacin and Yin Na in the methods of the invention, being prepared using the silver nano-particle solution of various concentration
The mixed solution of rice corpuscles is different for the enhancing effect of SERS signal, can be applied to it is a variety of in the case of Enrofloxacin inspection
It surveys.
4) it in the methods of the invention, is prepared using the carborundum paper of different meshes and under the conditions of different magnetron sputterings
Carborundum paper SERS substrates are different for the enhancing effect of SERS signal, can be applied to it is a variety of in the case of Enrofloxacin inspection
It surveys.
5) the carborundum paper SERS substrates that in the methods of the invention, are prepared using carborundum paper as template are flexible, can
Cut, be portable, preparation process is simple, it is of low cost, take that small, yield is high, it is easy to spread, convenient for application.
Description of the drawings
Fig. 1 a are the electricity for the carborundum paper SERS substrates that embodiment one is prepared using the carborundum paper of 2000 mesh
Sub- microscope photo；
The mixed solution of the Enrofloxacin and Nano silver grain that are obtained in the step of Fig. 1 b are embodiment one two is added drop-wise to
The Enrofloxacin obtained in the carborundum paper SERS substrates that the carborundum paper of 2000 mesh is prepared and after drying process
The electron micrograph of standard detection substrate (the small figure in the upper right corner is the Yin Na being distributed in carborundum paper SERS substrates
The electron micrograph of rice corpuscles)；
The standard detection substrate of the Enrofloxacin obtained in the step of Fig. 2 is SERS spectra figure, and curve 1 is embodiment one four
SERS spectra, obtained Enrofloxacin standard sample solution is directly added drop-wise to 2000 in the step of curve 2 is embodiment one two
Detection obtains on the substrate obtained after drying in the carborundum paper SERS substrates that purpose carborundum paper is prepared
The mixed solution of the Enrofloxacin and Nano silver grain that are obtained in the step of SERS spectra, curve 3 is embodiment one two is added drop-wise to
The SERS spectra detected on the substrate obtained after drying on quartz plate；
The standard detection substrate of the Enrofloxacin obtained in the step of Fig. 3 is SERS spectra figure, and curve 1 is embodiment one four
SERS spectra, curve 2 be extracted from the chicken containing Enrofloxacin detectable substance preparation Enrofloxacin base to be detected
The SERS spectra of piece, curve 3 are the base to be measured that Enrofloxacin prepared by detectable substance is extracted from the chicken without containing Enrofloxacin
The SERS spectra of piece；
Fig. 4 is the Enrofloxacin that the Enrofloxacin standard detection sample solution of various concentration is prepared in embodiment two
The SERS spectra that is detected of standard detection substrate；
Fig. 5 a are that the electron microscope for the SERS substrates that embodiment three is prepared using the carborundum paper of 800 mesh shines
Piece；
The mixed solution of the Enrofloxacin and Nano silver grain that are obtained in the step of Fig. 5 b are embodiment three two is added drop-wise to 800
The standard inspection of the Enrofloxacin obtained in carborundum paper SERS substrates prepared by purpose carborundum paper and after drying process
(the small figure in the upper right corner is the Nano silver grain being distributed in carborundum paper SERS substrates to the electron micrograph of survey substrate
Electron micrograph)；
The standard detection substrate of the Enrofloxacin obtained in the step of Fig. 6 is SERS spectra figure, and curve 1 is embodiment three four
SERS spectra, obtained Enrofloxacin standard sample solution is directly added drop-wise to 800 mesh in the step of curve 2 is embodiment three two
The carborundum paper SERS substrates that are prepared of carborundum paper on the SERS that detects on the substrate that obtains after drying
Spectrum；
Fig. 7 a are the electricity for the carborundum paper SERS substrates that example IV is prepared using the carborundum paper of 1200 mesh
Sub- microscope photo；
The mixed solution of the Enrofloxacin and Nano silver grain that are obtained in the step of Fig. 7 b are example IV two is added drop-wise to
The mark of the Enrofloxacin obtained in carborundum paper SERS substrates prepared by the carborundum paper of 1200 mesh and after drying process
(the small figure in the upper right corner is the nano grain of silver being distributed in carborundum paper SERS substrates to the electron micrograph of quasi- detection substrate
The electron micrograph of son)；
The standard detection substrate of the Enrofloxacin obtained in the step of Fig. 8 is SERS spectra figure, and curve 1 is example IV four
SERS spectra, obtained Enrofloxacin standard sample solution is directly added drop-wise to 1200 in the step of curve 2 is example IV two
The SERS light detected on the substrate obtained after drying in carborundum paper SERS substrates prepared by purpose carborundum paper
Spectrum；
Fig. 9 a are the electricity for the carborundum paper SERS substrates that embodiment five is prepared using the carborundum paper of 3000 mesh
Sub- microscope photo；
The mixed solution of the Enrofloxacin and Nano silver grain that are obtained in the step of Fig. 9 b are embodiment five two is added drop-wise to
The mark of the Enrofloxacin obtained in carborundum paper SERS substrates prepared by the carborundum paper of 3000 mesh and after drying process
(the small figure in the upper right corner is the nano grain of silver being distributed in carborundum paper SERS substrates to the electron micrograph of quasi- detection substrate
The electron micrograph of son)；
The standard detection base of the Enrofloxacin obtained in the step of Figure 10 is SERS spectra figure, and curve 1 is embodiment five four
The Enrofloxacin standard sample solution obtained in the step of SERS spectra of piece, curve 2 is embodiment five two is directly added drop-wise to
Detection obtains on the substrate obtained after drying in carborundum paper SERS substrates prepared by the carborundum paper of 3000 mesh
SERS spectra；
The SERS spectra that Figure 11 is detected on the standard detection substrate for the Enrofloxacin being prepared in embodiment six；
The SERS light that Figure 12 is detected on the standard detection substrate for the Enrofloxacin being prepared in embodiment seven
Spectrum；；
The SERS spectra that Figure 13 is detected on the standard detection substrate for the Enrofloxacin being prepared in embodiment eight.
Specific implementation mode
With reference to embodiments and its attached drawing present invention is further described in detail.
Embodiment one：
A kind of Enrofloxacin detection side based on nano-Ag particles Yu carborundum paper SERS substrates that the present embodiment proposes
Method examines Enrofloxacin in conjunction with Nano silver grain and the SERS substrates that the carborundum paper using 2000 mesh is prepared
It surveys, is as follows：
Step 1：300 microlitres of silver nano-particle solution is taken to inject centrifuge tube, then with 11000 revs/min of rotating speed pair
Silver nano-particle solution carries out eccentric cleaning, and cleaning removes supernatant after 30 minutes, retain the Yin Na for being deposited in centrifugation bottom of the tube
Rice corpuscles, then silver nanoparticle deposition object is suspended in 100 microlitres of the ethanol solution that mass percentage concentration is 50%, it obtains
The aaerosol solution of the monodispersed homogenous silver nano particle of a concentration of 360 mg/litre.
Here, the preparation process of silver nano-particle solution is：A1, a certain amount of analytically pure nitric acid silver powder is taken at room temperature
End, and be dissolved in deionized water and be stirred for uniformly obtaining the silver nitrate solution that mass percentage concentration is 0.018%；Then, right
The silver nitrate solution is heated to boiling while being stirred；A2, by a certain amount of analytically pure sodium citrate solution by
The mixing that the mass percent for being added dropwise in the silver nitrate solution of boiling, and persistently stirring to get sodium citrate is 0.06% is molten
Liquid cools down at room temperature until after the color of the mixed solution of boiling becomes celadon, and it is about 50 to receive to obtain monodispersed diameter
The homogenous silver nano particle solution of rice.
Step 2：The aaerosol solution of the monodispersed homogenous silver nano particle of 100 microlitres be prepared in step 1 is taken,
The Enrofloxacin powder by purity more than or equal to 98% is configured to the Enrofloxacin standard sample of a concentration of 5 mg/litre simultaneously
Then solution takes the Enrofloxacin standard sample solution of 150 microlitres of preparations and is added to 100 microlitres of monodispersed uniform silver and receives
The mixed solution of Enrofloxacin and Nano silver grain is mixed to form in the aaerosol solution of rice corpuscles, then to Enrofloxacin and silver nanoparticle
The mixed solution of particle be ultrasonically treated 10 minutes.
Step 3：The mixed solution for 40 microlitres of the Enrofloxacin and Nano silver grain that step 2 is prepared is taken, and is dripped
It is added in carborundum paper SERS substrates, is then dried at room temperature for, obtain the standard detection substrate of Enrofloxacin.
Here, the preparation process of carborundum paper SERS substrates is：The carborundum paper of 2000 mesh of regular shape is set
In rf magnetron sputtering system, and the operating pressure for controlling magnetic control sputtering system is 1.4 pas, and sputtering power is 50 watts, and
Deposition thickness is on carborundum paperSilver, obtain the carborundum paper SERS substrates using carborundum paper as template.
Step 4：Make that the power that laser emits is 30 milliwatts and laser beam that wavelength is 785 nanometers is through numerical aperture
Vertical irradiation is on the standard detection substrate of Enrofloxacin after 0.65 object lens focus, standard of the laser through Enrofloxacin of irradiation
It is received by Raman spectrometer after detection substrate reflection, Raman spectrometer shows the mark of Enrofloxacin after SERS spectra acquires 10 seconds
The SERS spectra of quasi- detection substrate.
Step 5：Before actually detected, according to document " A novel quantum dot-based
fluoroimmunoassay method for detection of Enrofloxacin residue in chicken
Muscle tissue, Food Chemistry, 2009, " (a kind of fluoroimmunoassay based on novel quantum dot is for examining
Survey remaining Enrofloxacin in Chicken Tissues, Food Chemistry, 2009) method of extraction detectable substance that provides, it is carried from 1 gram of chicken
It takes out detectable substance and is dissolved into 1 milliliter of mass percentage concentration to obtain detected sample solution in 50% ethanol solution, so
150 microlitres of the monodispersed homogenous silver nano grain that the detected sample solution of 225 microlitres of taking-up is prepared with step 1 afterwards
The mixed solution of Enrofloxacin and Nano silver grain is mixed to form in the aaerosol solution of son, then to Enrofloxacin and Nano silver grain
Mixed solution be ultrasonically treated learn from else's experience after ten minutes be ultrasonically treated after Enrofloxacin and Nano silver grain mixed solution
In the carborundum paper SERS substrates that 40 microlitres of carborundum papers for being added drop-wise to 2000 mesh are prepared, then it is dried at room temperature for,
Obtain the substrate to be detected of Enrofloxacin.
Step 6：Make that the power that laser emits is 30 milliwatts and laser beam that wavelength is 785 nanometers is through numerical aperture
Vertical irradiation is on the substrate to be detected of Enrofloxacin after 0.65 object lens focus, and the laser of irradiation is through Enrofloxacin base to be detected
It is received by Raman spectrometer after piece reflection, Raman spectrometer shows the base to be detected of Enrofloxacin after SERS spectra acquires 10 seconds
The SERS spectra of piece, and compared with the SERS spectra of the standard detection substrate of Enrofloxacin, if Enrofloxacin is to be checked
The SERS spectra for surveying substrate is identical as the SERS spectra of standard detection substrate of Enrofloxacin, then shows to contain in substrate to be detected
Contain Enrofloxacin in Enrofloxacin, that is, detectable substance；If the SERS spectra of the substrate to be detected of Enrofloxacin and grace fluorine
The SERS spectra of the standard detection substrate of Sha Xing differs, then shows not contain Enrofloxacin in detectable substance.
By the electronic display for the carborundum paper SERS substrates that the present embodiment is prepared using the carborundum paper of 2000 mesh
Micro mirror photo is as shown in Figure 1a.It can be seen that from FIG. 1 a that the size and spacing of the Argent grain being deposited on carborundum paper
It is 11 ± 5.4 microns in the size of micron dimension, particle, and shows many sharp corners, the silver-colored table of this thick grain
Face contributes to the enhancing of SERS signal.
The mixed solution of the Enrofloxacin and Nano silver grain that are obtained in the step of the present embodiment two is added drop-wise to the carbon of preparation
After in SiClx sand paper SERS substrates, the electron micrograph of Nano silver grain distribution thereon is as shown in Figure 1 b.From Fig. 1 b
As can be seen that apparent reunion is presented in Nano silver grain, to further enhance the intensity of SERS signal.
The SERS spectra of the standard detection substrate of the Enrofloxacin obtained in the step of embodiment one four is set forth in Fig. 2
The carborundum paper that the Enrofloxacin standard sample solution obtained in (curve 1) and step 2 is directly added drop-wise to 2000 mesh is prepared into
To carborundum paper SERS substrates on the SERS spectra (curve 2) that detects on the substrate that obtains after drying, Yi Jibu
The mixed solution of the Enrofloxacin and Nano silver grain that are obtained in rapid two is added drop-wise on the substrate obtained after drying on quartz plate
Detect obtained SERS spectra (curve 3).From figure 2 it can be seen that Enrofloxacin standard sample solution is directly added dropwise to carbonization
It does not detect Raman signal in silica sand paper SERS substrates, the mixed solution of Enrofloxacin and Nano silver grain is added dropwise to quartz plate
On only detect weak SERS signal, and strong SERS signal is detected by the standard detection substrate of Enrofloxacin,
1386cm-1The Raman signal intensity at place reaches 37118.Correlation curve 1 and curve 2, it can be seen that Nano silver grain for grace
The humidification of Flucloxacillin SERS signal, correlation curve 1 and curve 3, it can be seen that carborundum paper SERS substrates are for grace fluorine
The contribution of the enhancing of husky star SERS signal.
The SERS spectra of the standard detection substrate of the Enrofloxacin obtained in the step of embodiment one four is set forth in Fig. 3
(curve 1) and extracted from the chicken containing Enrofloxacin detectable substance preparation Enrofloxacin substrate to be detected SERS light
It composes (curve 2), and the substrate to be measured for the Enrofloxacin that from the chicken without containing Enrofloxacin prepared by extraction detectable substance
SERS spectra.Can clearly distinguish in chicken whether contain Enrofloxacin from Fig. 3.
Embodiment two：
The present embodiment proposes a kind of Enrofloxacin detection method based on nano-Ag particles Yu carborundum paper SERS substrates,
It combines Nano silver grain to be detected to Enrofloxacin with the SERS substrates that the carborundum paper using 2000 mesh is prepared.
The detection method to Enrofloxacin that the present embodiment provides the detection method and detection process of Enrofloxacin with embodiment one
And detection process is identical, the difference is that only that the present embodiment prepares grace fluorine used by the standard detection substrate of Enrofloxacin
The concentration of the husky quasi- sample solution of asterisk is different, and specifically the Enrofloxacin powder by purity more than or equal to 98% (HPLC) is prepared
It is respectively five kinds of Enrofloxacin standard sample solution of 0.01,0.05,0.1,0.5,1 mg/litre at concentration, then takes respectively
150 microlitres preparation various concentration Enrofloxacin standard sample solution and be added to five parts 100 microlitres it is monodispersed uniformly
The mixed solution of Enrofloxacin and Nano silver grain is respectively mixed to form in the aaerosol solution of Nano silver grain, then to five parts of grace fluorine
The mixed solution of Sha Xing and Nano silver grain carries out being ultrasonically treated 10 minutes respectively, then take respectively 40 microlitres of Enrofloxacin with
The mixed solution of Nano silver grain, and be added drop-wise in carborundum paper SERS substrates, five kinds of grace fluorine are obtained after being dried at room temperature for
The standard detection substrate of Sha Xing.
The result that the standard detection substrate of the Enrofloxacin of five kinds of various concentrations of preparation is detected by the present embodiment
As shown in figure 4, utilizing the Enrofloxacin detection method of the present invention husky for the grace fluorine of five kinds of various concentrations as can see from Figure 4
The standard detection substrate of star detects SERS signal, and detectable concentration can be as low as 0.01 mg/litre.
Embodiment three：
The present embodiment proposes a kind of Enrofloxacin detection method based on nano-Ag particles Yu carborundum paper SERS substrates,
It combines Nano silver grain to be detected to Enrofloxacin with the SERS substrates that the carborundum paper using 800 mesh is prepared.
The detection method to Enrofloxacin that the present embodiment provides the detection method and detection process of Enrofloxacin with embodiment one
And detection process is identical, the difference is that only that the present embodiment prepares the used silicon carbide of carborundum paper SERS substrates
The mesh number of sand paper is different, specifically uses the carborundum paper of 800 mesh that carborundum paper SERS substrates are prepared.
By the electron microscopic for the carborundum paper SERS substrates that the present embodiment is prepared using the carborundum paper of 800 mesh
Mirror photo is as shown in Figure 5 a.It can be seen from Fig. 5a that the size and spacing of the Argent grain being deposited on carborundum paper exist
The size of micron dimension, particle is 18.5 ± 9.8 microns, and shows many sharp corners, the silver-colored table of this thick grain
Face contributes to the enhancing of SERS signal.
The mixed solution of the Enrofloxacin and Nano silver grain that are obtained in the step of the present embodiment two is added drop-wise to the carbon of 800 mesh
After in carborundum paper SERS substrates prepared by SiClx sand paper, the electron micrograph of Nano silver grain distribution thereon is as schemed
Shown in 5b.It can be seen from figure 5b that apparent reunion is presented in Nano silver grain, to further enhance the strong of SERS signal
Degree.
The SERS spectra of the standard detection substrate of the Enrofloxacin obtained in the step of embodiment three four is set forth in Fig. 6
The carborundum paper that the Enrofloxacin standard sample solution obtained in (curve 1) and step 2 is directly added drop-wise to 800 mesh is prepared into
To carborundum paper SERS substrates on the SERS spectra (curve 2) that detects on the substrate that obtains after drying.From Fig. 6
Raman signal is not detected as can be seen that being directly added dropwise on Enrofloxacin solution to carborundum paper SERS substrates, and by grace
The standard detection substrate of Flucloxacillin detects strong SERS signal, in 1386cm-1The Raman signal intensity at place reaches 10819.
The Enrofloxacin detectable limit that the present embodiment can be extrapolated according to the detectable limit in embodiment two is about 0.034 mg/litre.
Example IV：
The present embodiment proposes a kind of Enrofloxacin detection method based on nano-Ag particles Yu carborundum paper SERS substrates,
It combines Nano silver grain to be detected to Enrofloxacin with the SERS substrates that the carborundum paper using 1200 mesh is prepared.
The detection method to Enrofloxacin that the present embodiment provides the detection method and detection process of Enrofloxacin with embodiment one
And detection process is identical, the difference is that only that the present embodiment prepares the used silicon carbide of carborundum paper SERS substrates
The mesh number of sand paper is different, specifically uses the carborundum paper of 1200 mesh that carborundum paper SERS substrates are prepared.
By the electronic display for the carborundum paper SERS substrates that the present embodiment is prepared using the carborundum paper of 1200 mesh
Micro mirror photo is as shown in Figure 7a.It can be seen from fig 7a that the size and spacing of the Argent grain being deposited on carborundum paper
It is 13.8 ± 7.5 microns in the size of micron dimension, particle, and shows many sharp corners, the silver of this thick grain
Surface contributes to the enhancing of SERS signal.
The mixed solution of the Enrofloxacin and Nano silver grain that are obtained in the step of the present embodiment two is added drop-wise to 1200 purposes
After in carborundum paper SERS substrates prepared by carborundum paper, the electron micrograph of Nano silver grain distribution thereon is such as
Shown in Fig. 7 b.As can be seen that apparent reunion is presented in Nano silver grain, to further enhance the strong of SERS signal from Fig. 7 b
Degree.
The SERS spectra of the standard detection substrate of the Enrofloxacin obtained in the step of example IV four is set forth in Fig. 8
The carborundum paper that the Enrofloxacin standard sample solution obtained in (curve 1) and step 2 is directly added drop-wise to 1200 mesh is prepared into
To carborundum paper SERS substrates on the SERS spectra (curve 2) that detects on the substrate that obtains after drying.From Fig. 8
Raman signal is not detected as can be seen that being directly added dropwise on Enrofloxacin solution to carborundum paper SERS substrates, and by grace
The standard detection substrate of Flucloxacillin detects strong SERS signal, in 1386cm-1The Raman signal intensity at place reaches 20569.
The Enrofloxacin detectable limit that the present embodiment can be extrapolated according to the detectable limit in embodiment two is about 0.018 mg/litre.
Embodiment five：
The present embodiment proposes a kind of Enrofloxacin detection method based on nano-Ag particles Yu carborundum paper SERS substrates,
It combines Nano silver grain to be detected to Enrofloxacin with the SERS substrates that the carborundum paper using 3000 mesh is prepared.
The detection method to Enrofloxacin that the present embodiment provides the detection method and detection process of Enrofloxacin with embodiment one
And detection process is identical, the difference is that only that the present embodiment prepares the used silicon carbide of carborundum paper SERS substrates
The mesh number of sand paper is different, specifically uses the carborundum paper of 3000 mesh that carborundum paper SERS substrates are prepared.
By the electronic display for the carborundum paper SERS substrates that the present embodiment is prepared using the carborundum paper of 3000 mesh
Micro mirror photo is as illustrated in fig. 9.As can be seen that the size and spacing of the Argent grain being deposited on carborundum paper from Fig. 9 a
It is 6.7 ± 2.7 microns in the size of micron dimension, particle, and shows many sharp corners, the silver-colored table of this thick grain
Face contributes to the enhancing of SERS signal.
The mixed solution of the Enrofloxacin and Nano silver grain that are obtained in the step of the present embodiment two is added drop-wise to 3000 purposes
After in carborundum paper SERS substrates prepared by carborundum paper, the electron micrograph of Nano silver grain distribution thereon is such as
Shown in Fig. 9 b.As can be seen that apparent reunion is presented in Nano silver grain, to further enhance the strong of SERS signal from Fig. 9 b
Degree.
The SERS light of the standard detection substrate of the Enrofloxacin obtained in the step of embodiment five four is set forth in Figure 10
It is prepared by the carborundum paper that the Enrofloxacin standard sample solution obtained in spectrum (curve 1) and step 2 is directly added drop-wise to 3000 mesh
The SERS spectra (curve 2) detected on the substrate obtained after drying in obtained carborundum paper SERS substrates.From figure
In 10 Raman signal is not detected as can be seen that being directly added dropwise on Enrofloxacin solution to carborundum paper SERS substrates, and
Strong SERS signal is detected by the standard detection substrate of Enrofloxacin, in 1386cm-1The Raman signal intensity at place reaches
17981.The Enrofloxacin detectable limit that the present embodiment can be extrapolated according to the detectable limit in embodiment two is about 0.021 milli
Grams per liter.
The Enrofloxacin detection method that comparing embodiment one, embodiment three, example IV and embodiment five provide detects
The Surface Enhanced Raman Scattering Spectrum of the Enrofloxacin arrived, it can be seen that the carborundum paper SERS substrates of different meshes are for grace
The Raman signal intensity of Flucloxacillin has a certain impact, and the grace detected when carborundum paper SERS substrates are 2000 mesh
The Raman signal of Flucloxacillin is most strong.
Embodiment six：
A kind of Enrofloxacin detection side based on nano-Ag particles Yu carborundum paper SERS substrates that the present embodiment proposes
Method, the Enrofloxacin detection method proposed with embodiment one is the difference is that step 1, i.e.,：Make silver nanoparticle deposition
In the ethanol solution that the mass percentage concentration that object is suspended in 300 microlitres is 50%, the monodisperse of a concentration of 120 mg/litre is formed
Homogenous silver nano particle aaerosol solution.
The SERS spectra such as Figure 11 institutes detected on the standard detection substrate for the Enrofloxacin that the present embodiment is prepared
Show.The power of laser used is 30 milliwatts when detection, and SERS spectra acquisition time is 10 seconds.It can be seen from fig. 11 that by this
The standard detection substrate of embodiment detection Enrofloxacin obtains stronger SERS signal, in 1386cm-1The Raman signal at place is strong
Degree reaches 11673.
Embodiment seven：
A kind of Enrofloxacin detection side based on nano-Ag particles Yu carborundum paper SERS substrates that the present embodiment proposes
Method, the Enrofloxacin detection method proposed with embodiment one is the difference is that step 1, i.e.,：Make silver nanoparticle deposition
In the ethanol solution that the mass percentage concentration that object is suspended in 150 microlitres is 50%, the monodisperse of a concentration of 240 mg/litre is formed
Homogenous silver nano particle aaerosol solution.
The SERS spectra such as Figure 12 institutes detected on the standard detection substrate for the Enrofloxacin that the present embodiment is prepared
Show.The power of laser used is 30 milliwatts when detection, and SERS spectra acquisition time is 10 seconds.In figure 12 it can be seen that this reality
The standard detection substrate for applying example detection Enrofloxacin obtains stronger SERS signal, in 1386cm-1The Raman signal intensity at place
Reach 17316.
Embodiment eight：
A kind of Enrofloxacin detection side based on nano-Ag particles Yu carborundum paper SERS substrates that the present embodiment proposes
Method, the Enrofloxacin detection method proposed with embodiment one is the difference is that step 1, i.e.,：Make silver nanoparticle deposition
In the ethanol solution that the mass percentage concentration that object is suspended in 75 microlitres is 50%, the monodispersed of a concentration of 480 mg/litre is formed
The aaerosol solution of homogenous silver nano particle.
The SERS spectra such as Figure 13 institutes detected on the standard detection substrate for the Enrofloxacin that the present embodiment is prepared
Show.The power of laser used is 30 milliwatts when detection, and SERS spectra acquisition time is 10 seconds.It can be observed from fig. 13 that this reality
The standard detection substrate for applying example detection Enrofloxacin obtains strong SERS signal, in 1386cm-1The Raman signal intensity at place reaches
To 25326.
The Enrofloxacin detection method that comparative example one, embodiment six, embodiment seven and embodiment eight provide detects
The Surface Enhanced Raman Scattering Spectrum arrived has been found that while stronger SERS signal, but the grace fluorine that embodiment one provides is husky
The SERS signal that star detection method detects is most strong, therefore by 300 microlitres of Yin Na in embodiment two to embodiment five
Silver nanoparticle deposition object after the centrifugation of rice corpuscles solution is suspended in 100 microlitres of the ethanol solution that mass percentage concentration is 50%
In.
Claims (6)
1. a kind of Enrofloxacin detection method based on nano-Ag particles Yu carborundum paper SERS substrates, it is characterised in that in conjunction with
Nano-Ag particles are detected Enrofloxacin with carborundum paper SERS substrates, are as follows：
Step 1：It takes silver nano-particle solution to inject centrifuge tube, eccentric cleaning then is carried out to silver nano-particle solution, is then existed
It removes supernatant after eccentric cleaning, retains the Nano silver grain for being deposited in centrifugation bottom of the tube, then by silver nanoparticle deposition
Object is suspended in the ethanol solution that mass percentage concentration is 50%, obtains the aaerosol solution of monodispersed homogenous silver nano particle；
The preparation process of silver nano-particle solution is in the step one：A1, analytically pure silver nitrate powder is taken at room temperature,
And it is dissolved in deionized water and is stirred for uniformly obtaining the silver nitrate solution that mass percentage concentration is 0.009%~0.018%；
Then it is heated to boiling while being stirred silver nitrate solution；A2, analytically pure sodium citrate solution is added dropwise to
In the silver nitrate solution of boiling, and the mixing that the mass percent for persistently stirring to get sodium citrate is 0.03%~0.06% is molten
Liquid cools down until after the color of the mixed solution of boiling becomes celadon, obtains monodispersed a diameter of 25~80 at room temperature
The homogenous silver nano particle solution of nanometer；
Step 2：The aaerosol solution for the monodispersed homogenous silver nano particle being prepared in step 1 is taken, while purity is big
The Enrofloxacin standard sample solution of a concentration of 0.01~5 mg/litre is configured in or equal to 98% Enrofloxacin powder, so
Enrofloxacin standard sample solution is added to afterwards in the aaerosol solution of the monodispersed homogenous silver nano particle taken and mixes shape
It is carried out at ultrasound at the mixed solution of Enrofloxacin and Nano silver grain, then to the mixed solution of Enrofloxacin and Nano silver grain
Reason；
Step 3：The mixed solution for the Enrofloxacin and Nano silver grain that step 2 is prepared is taken, and is added drop-wise to silicon carbide sand
It in paper SERS substrates, then is dried at room temperature for, obtains the standard detection substrate of Enrofloxacin；
Step 4：Vertical irradiation is irradiated on the standard detection substrate of Enrofloxacin after making the laser line focus of laser transmitting
Laser received by Raman spectrometer after the standard detection substrate reflection of Enrofloxacin, Raman spectrometer shows Enrofloxacin
Standard detection substrate SERS spectra；
Step 5：Before actually detected, detectable substance is extracted, and dissolve detectable substance and obtain detected sample solution；Then step 1 is taken
In the aaerosol solution of monodispersed homogenous silver nano particle that is prepared；Then the detected sample solution of preparation is added to
It is mixed to form Enrofloxacin in the aaerosol solution of the monodispersed homogenous silver nano particle taken and the mixing of Nano silver grain is molten
Liquid, then the mixed solution of Enrofloxacin and Nano silver grain is ultrasonically treated；Grace fluorine after later will be sonicated is husky
The mixed solution of star and Nano silver grain is added drop-wise in carborundum paper SERS substrates, then is dried at room temperature for, and it is husky to obtain grace fluorine
The substrate to be detected of star；
Step 6：When actually detected, vertical irradiation is in the base to be detected of Enrofloxacin after making the laser line focus of laser transmitting
The laser of on piece, irradiation is received after the substrate reflection to be detected of Enrofloxacin by Raman spectrometer, and Raman spectrometer is shown
The SERS spectra of the substrate to be detected of Enrofloxacin；Then the SERS spectra and grace fluorine of the standard detection substrate of Enrofloxacin are compared
The SERS spectra of the substrate to be detected of Sha Xing, if the standard of the SERS spectra and Enrofloxacin of the substrate to be detected of Enrofloxacin
The SERS spectra for detecting substrate is identical, then shows to contain Enrofloxacin in the substrate to be detected of Enrofloxacin, that is, show detectable substance
In contain Enrofloxacin；If the SERS spectra of the substrate to be detected of Enrofloxacin and the standard detection substrate of Enrofloxacin
SERS spectra differs, then shows not contain Enrofloxacin in the substrate to be detected of Enrofloxacin, that is, show not contain in detectable substance
There is Enrofloxacin；
The preparation process of carborundum paper SERS substrates is in the step three and the step five：By the carbon of regular shape
SiClx sand paper is placed in rf magnetron sputtering system, and the operating pressure for controlling magnetic control sputtering system is 0.1~1.4 pa, sputtering
Power is 50~150 watts, and deposition thickness is on carborundum paperSilver, obtain be with carborundum paper
The mesh number of the carborundum paper SERS substrates of template, above-mentioned carborundum paper is 240~5000 mesh.
2. the Enrofloxacin detection side according to claim 1 based on nano-Ag particles Yu carborundum paper SERS substrates
Method, it is characterised in that ranging from 100~500 microlitres of institute's taken amount of silver nano-particle solution in the step one；Described
Ranging from 25~500 microlitres of institute's taken amount of ethanol solution in step 1；Enrofloxacin standard sample is molten in the step two
Ranging from 25~150 microlitres of institute's taken amount of liquid；The mixed solution of Enrofloxacin and Nano silver grain in the step three
Ranging from 25~50 microlitres of institute's taken amount.
3. the Enrofloxacin according to claim 1 or 2 based on nano-Ag particles and carborundum paper SERS substrates detects
Method, it is characterised in that the rotating speed for carrying out eccentric cleaning in the step one to silver nano-particle solution is 5000~11000
Rev/min, scavenging period be 5~30 minutes.
4. the Enrofloxacin detection side according to claim 3 based on nano-Ag particles Yu carborundum paper SERS substrates
Method, it is characterised in that the processing that the mixed solution of Enrofloxacin and Nano silver grain is ultrasonically treated in the step two
Time is 10~30 minutes.
5. the Enrofloxacin detection side according to claim 1 based on nano-Ag particles Yu carborundum paper SERS substrates
Method, it is characterised in that the time of integration that SERS spectra is acquired in the step four and the step six is 1~10 second, irradiation
The power of laser is 3~30 milliwatts, and optical maser wavelength is 785 nanometers.
6. the Enrofloxacin detection side according to claim 1 based on nano-Ag particles Yu carborundum paper SERS substrates
Method, it is characterised in that the suspension of detected sample solution and the monodispersed homogenous silver nano particle taken in the step five
The volume ratio of solution is 3：2；The processing time of supersound process is 10~30 minutes；Enrofloxacin after sonicated and Yin Na
Institute's taken amount of the mixed solution of rice corpuscles is 25~50 microlitres.
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