CN108444971A - Remaining paper substrate chip of pesticide and its preparation method and application in a kind of detection fruits and vegetables - Google Patents
Remaining paper substrate chip of pesticide and its preparation method and application in a kind of detection fruits and vegetables Download PDFInfo
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- CN108444971A CN108444971A CN201810226435.6A CN201810226435A CN108444971A CN 108444971 A CN108444971 A CN 108444971A CN 201810226435 A CN201810226435 A CN 201810226435A CN 108444971 A CN108444971 A CN 108444971A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N2021/653—Coherent methods [CARS]
- G01N2021/655—Stimulated Raman
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Abstract
The invention discloses remaining paper substrate chips of pesticide in a kind of detection fruits and vegetables and its preparation method and application.It is as follows：(1) fulmargin is prepared by reduction of sodium citrate method；(2) hydrazine hydrate reduction graphene oxide is utilized, graphene solution is prepared；(3) graphene solution is injected into print cartridge, prints different number of plies graphenes on paper by ink-jet printer, obtain graphene test paper substrate；(4) fulmargin is injected into print cartridge, different layers of silver nano-grains is printed in graphene test paper substrate by ink-jet printer, prepare the remaining paper substrate chip of pesticide in detection fruits and vegetables.Preparation method of the present invention is simple, by the way that fruit and vegetable surfaces simple wiping, quickly by pesticide residue Molecular Adsorption in surface, and then qualitative and quantitative detection agriculture is residual, and detection limit is low, has in the rapid and convenient detection of fruits and vegetables and has great advantage.
Description
Technical field
The invention belongs to the Detection Technologies of Pesticide Residues fields, specifically, it is remaining to be related to pesticide in a kind of detection fruits and vegetables
Paper substrate chip and its preparation method and application.
Background technology
Pesticide residue refers to that applying pesticides rear portion pesticide directly or indirectly remains in cereal, vegetable in agricultural production
Phenomenon in dish, fruit, livestock products, aquatic products and in soil and water body.The pesticide being applied on crop, a portion are attached
It on crop, a part is scattered in the environment such as soil, air and water, and the part in the pesticide of environment remaining can be planted again
Object absorbs.According to the survey showed that, caused by the high fruits and vegetables of the mainly edible persticide residue of collectively in part food poisoning.
Therefore the pesticide residue in fruits and vegetables has become the major issue for endangering environment and health.Traditional pesticide is remaining
Rapid detection method includes the methods of enzyme-linked immunosorbent assay (ELISA), enzyme inhibition, these detection methods have pretreatment fiber crops
It is tired of, detection limits the deficiencies of not high, a kind of quick, high sensitivity modern measure method of urgent need exploitation.
In recent years, a kind of surface-enhanced Raman (SERS) spectral technique based on noble metal substrate causes the wide of researcher
General interest.SERS technologies since it is highly sensitive, limits low advantage without destructive, detection, be widely used in detecting biomolecule,
The fields such as food additives, environmental science.Usually effectively enhance SERS signal by two methods：When structure stabilization,
Highly sensitive and controllable SERS substrates；Second is that by by sample preconcentration technology and SERS combinations, the special of detection object is realized
Type adsorbs and detection.However traditional base material is rigid and smooth, such as glass slide or silicon wafer, this material have
The shortcomings of preparation process is complicated, detection narrow application range.In addition, being stablized by the SERS active-substrate that nanofabrication technique produces
Property it is poor, affected by environment big, therefore, exploitation is a kind of simple for production, easy to use and has highly sensitive and high stability SERS bases
Bottom is significant.
Invention content
In order to overcome the deficiencies of above-mentioned traditional Raman substrate material preparation is cumbersome, poor for applicability and stability is poor, the present invention
Provide remaining paper substrate chip of pesticide and its preparation method and application in a kind of detection fruits and vegetables.The present invention passes through inkjet printing skill
Graphene and Nano silver grain are printed upon on cellulosic filter paper to prepare Raman substrate material, the porous structure of paper substrate by art
Natural characterization of adsorption is provided, the separation and enrichment of analysis ingredient are used for, difference can be prepared by adjusting print pass
The enhancing base material of concentration；There is flexible and height Raman active feature by Raman substrate material prepared by inkjet printing,
There is important value to the analysis of biomolecule detection, environmental area.
Technical scheme of the present invention is specifically described as follows.
The preparation method of the remaining paper substrate chip of pesticide, is as follows in a kind of detection fruits and vegetables：
(1) fulmargin is prepared by reduction of sodium citrate method；
(2) hydrazine hydrate reduction graphene oxide is utilized, graphene solution is prepared；
(3) graphene solution is injected into print cartridge, prints different number of plies graphenes on paper by ink-jet printer, obtains stone
Black alkene test paper substrate；
(4) fulmargin is injected into print cartridge, is printed in graphene test paper substrate by ink-jet printer different layers of
Silver nano-grain prepares the remaining paper substrate chip of pesticide in detection fruits and vegetables.
In the present invention, in step (1), the mass-volume concentration of fulmargin is 6 × 10-2-10×10-2mg/mL；Elargol
The grain size of silver nano-grain is between 10-40nm in solution.
In the present invention, in step (2), the mass-volume concentration of graphene solution is 0.5-2mg/mL.
In the present invention, in step (3), paper is cellulosic filter paper；Editor's printing curve is long 2.5-3.5cm, wide 0.5-
The rectangle of 2.5cm.
In the present invention, in step (3), the number of plies for printing graphene is 1-5 layers.
In the present invention, in step (3), the number of plies for printing graphene is 1-3 layers.
In the present invention, in step (4), the number of plies for printing silver nano-grain is 1-3 layers.
In the present invention, pesticide is any one or several in thiram, probenazole or parathion-methyl.
The present invention also provides the remaining paper substrate chip of pesticide in fruits and vegetables is detected made from a kind of above-mentioned preparation method.
The present invention further provides the remaining paper substrate chips of pesticide in a kind of above-mentioned detection fruits and vegetables in detection fruits and vegetables middle peasant
Application in terms of medicine residual is first used paper substrate chip to wipe fruit and vegetable surfaces, then is realized in fruits and vegetables by surface Raman enhancement spectrum
The qualitatively and quantitatively detection of pesticide residue.
Compared with prior art, the beneficial effects of the present invention are：
1, used in the present invention is common paper as base material, and it is special that the porous structure of paper substrate provides natural absorption
Property, it can be used for the separation and enrichment of analysis ingredient, while for the load of material；Enhancing in Raman detection compared to conventional surface makes
Silicon wafer has many advantages, such as cheap and prepares easy.
2, the present invention prepares graphene-silver test paper composite reinforcing material using inkjet printing technology, and graphene is a kind of list
Layer carbon atom close-packed arrays, the two-dimentional graphite for forming cellular crystal structure, this structure have good absorption property, in addition
Due to its prodigious specific surface area so having very high sensitivity in adatom or molecule, and the nano grain of silver prepared
Sub- rough surface, plasma resonance has been allowed to higher enhancement factor under excitation light source irradiation.Change simultaneously the printing of test paper
Number, reaches the concentration control to Argent grain, and obtained nano material has good controllability and sensitivity.
3, the present invention can be used for the analysis inspection of solid or solution example with standby graphene-Yin Laman reinforcing materials made of paper
Survey, can realize the residual quick detection of surface agriculture of the samples such as fruits and vegetables by wipe method, have extensibility it is good, it is easy to operate, using model
Enclose the advantages that wide.
Description of the drawings
Fig. 1 is the optics picture that inkjet printing technology prepares composite material in embodiment 1.
Fig. 2 is the scanning electron microscope diagram that single-layer graphene-silver composite material is prepared in embodiment 1.
Fig. 3 is the scanning electron microscope diagram that multi-layer graphene-silver composite material is prepared in embodiment 1.
Fig. 4 is the activity figure of the four kinds of graphene-silver composite materials prepared in embodiment 1.
Fig. 5 is the Raman spectrogram of three standard sample of pesticide in embodiment 1.
Fig. 6 is that the practical remaining Raman spectrogram of fruits and vegetables is detected in application examples 1.
Specific implementation mode
It describes in detail with reference to the accompanying drawings and examples to technical scheme of the present invention.
Embodiment 1
(1) fulmargin is prepared
At ambient temperature, 40ml glycerine and 60ml deionized waters are measured in three-necked flask, uniform stirring is to having mixed
Entirely.95 DEG C are slowly heated in the case of reflux.It waits for that temperature is stablized at 95 DEG C, rapidly joins AgNO3Solution (prepares 18mgAgNO3In
2ml water), sodium citrate solution (prepare 60mg sodium citrates and be dissolved in 4ml water) is added after 1-2min, this temperature is kept at 95 DEG C
Spend 1h.For one hour postcooling to room temperature, 8000r is centrifuged off extra sodium citrate, and distilled water washs, and last obtained 9.22
×10-2The silver sol of mg/mL is sealed in 4 DEG C of preservations, and Argent grain grain size is between 20-30nm.
(2) reduction of graphene oxide water solution
At ambient temperature, 5ml graphene oxide water solutions (2mg/ml), 5ml hydrazine hydrates are added in three-necked flask
(35%), it is sufficiently stirred, adds 100 μ l ammonium hydroxide (28%), uniform stirring is heated to 95 DEG C, reacts 1h, is cooled to room temperature.
Different layers of graphenes are screened in 10000r centrifugations, prepare the graphene solution of the 1mg/ml of favorable dispersibility, close
It is encapsulated in 4 DEG C of preservations.
(3) inkjet printing prepares SERS activity test paper materials
Ink-jet printer is chosen as the printer device for preparing test paper base material, we use Epson stylus
T10 printers, resolution ratio are 5760 × 1440.The silver sol of preparation and graphene solution are injected separately into print cartridge, compiled with figure
Device print from the definition pattern is collected, test paper shape is designed.Since the detection method of the present invention is wiped with active paper obtained
Fruit and vegetable surfaces absorption pesticide residue molecule to be measured is wiped, Raman detection is carried out to reach testing requirements to active paper, so printing
Pattern influences test smaller.Herein, we edit print pattern as long 2.5cm, and the rectangle of wide 1.5cm, this shape exists
It is also to facilitate cutting and carrying in detection process.We first, it is respectively single layer and 3 layers of graphite that the number of plies is printed in base paper
Alkene is single layer and 3 layers of silver sol, optics picture in printing the number of plies on different layers of graphene test paper after abundant drying
As shown in Figure 1.Due to can freely design test paper shape, the ink jet printing method of the present invention, which prepares base material, has operation
Simply, it is suitble to the advantages that mass production.Simultaneously by regulating and controlling printing times, the graphite of various concentration elargol can be prepared
Alkene-human lymph node composite material, Fig. 2 and Fig. 3 are that the scanning electron for the graphene test paper material for printing single layer and 3 layers of elargol is aobvious respectively
The silver nano-grain of micro mirror figure, printing is uniformly scattered in graphene test paper base material, and graphene can be effectively as plane base
Bottom and sorbing material.It is proved simultaneously by comparing, the regulation and control printing number of plies can be effectively increased the concentration of silver ion, to screen
The maximum silver concentration of enhancement factor has been provided, to the largest optimization of graphene-silver test paper composite material, and then a nanometer material can have been reached
Prepared by the controllability of material, controllably change to nano material and uniform research direction and propose important construction meaning.We use ATP
As probe molecule, single layer elargol/three layers of silver glue, three layer graphenes is added to add single layer elargol/tri- layer the single-layer graphene of printing
These four materials of elargol carry out active comparison, it is found that single-layer graphene adds three layers of silver glue to have best sensitivity such as Fig. 4.
(4) to different pesticide qualitative and quantitative detections
Three kinds of parathion-methyl, thiram, probenazole standard sample of pesticide are prepared into a series of concentration gradient 0-100mM,
10 μ L analyte solutions are added dropwise on graphene-silver test paper material, then glass slide is placed on to the laser mirror of Raman spectrometer
Under head, excitation wavelength 785nm is opened optical camera, is focused using white light, reach maximum resolution.Raman is adjusted again
The time of integration is 10000ms, laser intensity 10mW.It chooses 100mM thiram concentration and tries printing different layers of graphenes-silver
Paper material carries out the characteristic peak analysis of thiram, investigates the SERS activity of the different elargol numbers of plies, determines best concentration ratio.By
Experiment find printing single-layer graphene and 3 layers of fulmargin filter paper material have good sensitivity, as a result with embodiment 1
(2) result obtained using ATP as probe molecule in is consistent, because the increase by graphene number of plies reduces material instead
SERS sensitivity, reason are that too strong adsorptivity is Nano silver grain aggregation and reduces the specific surface area contacted with analyte.With
The pesticide of various concentration is detected successively afterwards, studies the characteristic peak of three kinds of analytes, qualitative and quantitative inspection is carried out to pesticide
Analysis is surveyed, while investigating out the minimum detection of parathion-methyl and being limited to 10-7Mol/L, thiram and probenazole detection are limited to 10-6,
Such as Fig. 4, by the Raman spectrum map analysis to three kinds of pesticides, each of which pesticide has oneself characteristic peak, in this way to actually detected
Qualitative it can distinguish different types of pesticide residue.
Application examples 1
It is right by the graphene-Yin Laman reinforcing materials obtained of success in embodiment 1 for the actually detected of fruits and vegetables
The remaining quantitative and qualitative detection of pesticide, the single-layer graphene that we use above-mentioned SERS effects best herein in fruits and vegetables
Add the graphene-Yin Laman reinforcing materials of 3 layers of fulmargin.
Fruits and vegetables sample is being picked on the spot, it is known that the fruits and vegetables sample picked had been sprayed pesticide, and in farm chemical ingredients
Contain the ingredient to be detected.To keep the reset condition of sample, wearing gloves simultaneously to be moulded in the case where not contacting sample surfaces
Material protective case keeps sample and to be put into refrigerator cold-storage spare.What is chosen herein is four kinds of apple, banana, eggplant, Chinese cabbage differences
Fruits and vegetables.When detecting, since the base material of preparation is applicable to the sampling of complex surface, in the feelings for not cutting fruits and vegetables
Under condition, directly pesticide residue is extracted in complete fruit and vegetable surfaces with the active paper prepared.In extraction, directly in fruit and vegetable dryness table
Face directly wipes, and active paper surface is made fully to adsorb the residual molecule of agriculture, then carries out Raman spectrum acquisition to the active paper for having agriculture residual.
First, active paper is placed on glass slide, it is 10000ms, laser to select excitation wavelength 785nm, the adjusting Raman time of integration
Intensity 10mW.Apple, banana, eggplant, Chinese cabbage are detected successively, Raman spectrogram as shown in Figure 5, apple, banana, eggplant
Son, Chinese cabbage can all have pesticide residue ingredient, and concentration reaches a μm ol/L ranks, has to health, Environmental security etc. important
Harm.Known limited Pesticides Testing in apple and Banana peel using G-SERS methods is respectively 1.6ng/cm2And 10ng/
cm2；Using method associated with liquid chromatogram and tandem mass spectrum to the detection of eggplant and Chinese cabbage be limited to 0.0012mg/kg and
0.03mg/kg.It can thus be concluded that the present invention also has the advantages that sensitivity is high other than detecting quick and convenient advantage, in practical agriculture
It is made great sense in residual detection.
Claims (10)
1. the preparation method of the remaining paper substrate chip of pesticide in a kind of detection fruits and vegetables, which is characterized in that be as follows：
(1) fulmargin is prepared by reduction of sodium citrate method；
(2) hydrazine hydrate reduction graphene oxide is utilized, graphene solution is prepared；
(3) graphene solution is injected into print cartridge, prints different number of plies graphenes on paper by ink-jet printer, obtains graphene
Test paper substrate；
(4) fulmargin is injected into print cartridge, printing different layers of silver in graphene test paper substrate by ink-jet printer receives
Rice grain prepares the remaining paper substrate chip of pesticide in detection fruits and vegetables.
2. preparation method according to claim 1, which is characterized in that in step (1), the mass-volume concentration of fulmargin
It is 6 × 10-2-10×10-2mg/mL；The grain size of silver nano-grain is between 10-40nm in fulmargin.
3. preparation method according to claim 1, which is characterized in that in step (2), the quality volume of graphene solution is dense
Degree is 0.5-2mg/mL.
4. preparation method according to claim 1, which is characterized in that in step (3), paper is cellulosic filter paper；Editor beats
Impression shape is long 2.5-3.5cm, the rectangle of wide 0.5-2.5cm.
5. preparation method according to claim 1, which is characterized in that in step (3), the number of plies for printing graphene is respectively
1-5 layers.
6. preparation method according to claim 1 or 5, which is characterized in that in step (3), the number of plies for printing graphene is
1-3 layers.
7. preparation method according to claim 1, which is characterized in that in step (4), the number of plies for printing silver nano-grain is
1-3 layers.
8. preparation method according to claim 1, which is characterized in that pesticide is thiram, probenazole or parathion-methyl
In it is any one or several.
9. the remaining paper substrate chip of pesticide in a kind of preparation method according to claim 1 detection fruits and vegetables obtained.
10. the remaining paper substrate chip of pesticide pesticide in detecting fruits and vegetables is residual in a kind of detection fruits and vegetables according to claim 9
Stay the application of aspect, which is characterized in that it first uses paper substrate chip to wipe fruit and vegetable surfaces, then is realized by surface Raman enhancement spectrum
Pesticide is remaining in fruits and vegetables qualitatively and quantitatively detects.
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| CN201810226435.6A CN108444971A (en) | 2018-03-19 | 2018-03-19 | Remaining paper substrate chip of pesticide and its preparation method and application in a kind of detection fruits and vegetables |
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Cited By (7)
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| CN110441282A (en) * | 2019-07-19 | 2019-11-12 | 盐城工学院 | A kind of Pesticide Residues in Tea detection method based on Surface enhanced Raman spectroscopy and papery micro-fluidic chip |
| CN110579463A (en) * | 2019-10-09 | 2019-12-17 | 江南大学 | Surface-enhanced Raman flexible substrate for quantitative detection of pesticide methyl parathion and detection method |
| CN111208131A (en) * | 2018-11-21 | 2020-05-29 | 中国科学院大连化学物理研究所 | Array type high-precision pH test paper based on ink-jet printing technology |
| CN111208113A (en) * | 2020-02-28 | 2020-05-29 | 中国地质大学（北京） | Self-powered SERS substrate based on flexible piezoelectric film loaded with nano Ag and application |
| CN112986214A (en) * | 2021-03-14 | 2021-06-18 | 闽江学院 | Preparation method of flexible substrate for quantitatively detecting pesticide residues |
| CN114199850A (en) * | 2021-11-11 | 2022-03-18 | 江苏大学 | Method for detecting three food-borne pathogenic bacteria based on Au @ Ag NPs filter paper substrate |
| CN114609117A (en) * | 2022-02-24 | 2022-06-10 | 山西农业大学 | Preparation method and application of SERS substrate nondestructive testing test paper of nanogold triangle @ fiber membrane material |
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| CN114609117A (en) * | 2022-02-24 | 2022-06-10 | 山西农业大学 | Preparation method and application of SERS substrate nondestructive testing test paper of nanogold triangle @ fiber membrane material |
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Application publication date: 20180824 |