CN106970138A - The paper substrate of metal oxide nanoparticles modification and its application in sample detection - Google Patents
The paper substrate of metal oxide nanoparticles modification and its application in sample detection Download PDFInfo
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Abstract
The invention discloses a kind of paper substrate of metal oxide nanoparticles modification and its application in sample detection, the preparation method of metal oxide nanoparticles, the paper substrate that metal oxide nanoparticles are modified, the preparation method of the paper substrate of metal oxide nanoparticles modification, the application of the paper substrate of metal oxide nanoparticles modification are specifically included.The method that the paper substrate of metal oxide nanoparticles modification of the present invention is used for sample detection has the advantages that with low cost, easy to operate, Detection results are good, can realize quick detection.
Description
Technical field
The present invention relates to a kind of paper substrate of metal oxide nanoparticles modification, and in particular to one kind includes Co3O4Nanometer
The synthesis of grain, Co3O4Nano-particle modified paper substrate and its application in sample detection.
Background technology
China is global maximum toy manufacturing nation and exported country, and the toy in the whole world nearly 70% is made in China.However, playing
Tool industry is triggered while accelerating China's economic development and providing rich and varied life to numerous children by unqualified toy
Quality safety event also often occurs.The poisonous and harmful substance added in toy product can by swallowing, licking, skin contact,
The modes such as eye contact, suction enter in children's body, grave danger children's health.In dyeing course, dye molecule is by inhaling
Attached, diffusion etc. is a variety of chemically or physically to be handled, and is transferred to from dye liquor on pollutant and is allowed to dye.According to European Committee for Standardization
Requirement of the EN71 toy safeties series standard of formulation to toy chemical property, alkaline purple 1, disperse blue 106, alkalescence red 9 is disperseed
Indigo plant 1, disperse orange 3, solvent yellow 1, solvent yellow 2, disperse blue 124, disperse yellow 3, disperse orange 37, Red-1 200, solvent yellow 3, alkalescence purple
3 grade dyestuffs must not be detected in toy product.
At present, the method for dyestuff mainly has high performance liquid chromatography, gas chromatography-mass spectrography etc. in detection toy, these
Method respectively has advantage, but mostly instrument is heavy, cumbersome, it is impossible to the need for meeting on-site quick screening.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of with low cost, easy to operate, Detection results it is good, can realize
The paper substrate of the metal oxide nanoparticles modification of quick detection and its application in sample detection.
A kind of preparation method of metal oxide nanoparticles, comprises the following steps：
By the Co (CH that 25mL concentration is 0.4M3CO2)2·4H2O sample is added in the urea that 50mL concentration is 0.8M, is stirred
Mix after 30 minutes, in the stainless steel autoclave for transferring the solution into teflon back boxing, and placement 10 is small under 100 DEG C of constant temperatures
When；Resulting sediment is washed with deionized three times, and dried 30 minutes at 60 DEG C；Finally, by from room temperature with 1
DEG C/min speed is warming up to 400 DEG C and kept for 80 minutes under the conditions of 400 DEG C, calcining obtains Co3O4Nano particle.
A kind of paper substrate of metal oxide nanoparticles modification, wherein, including Co of the present invention3O4Nano particle.
The preparation method of the paper substrate of metal oxide nanoparticles modification of the present invention, comprises the following steps：
Weigh the obtained Co3O40.5~1g of nano particle, after grinding 20~30 minutes, with 30~50mL absolute ethyl alcohols
It is scattered, and stir 10~20 minutes, obtain Co3O4Dispersion liquid, chromatographic paper is laid on flat polytetrafluoroethylene, institute
Stating has uniform space to be used for filtering solution under polytetrafluoroethylene, by the Co3O4Homogeneous dispersion is scattered in described poly- four
On fluoride flat, 8~10 hours are stood at room temperature, treats that ethanol solution volatilizees completely, obtains dry metal oxide
Nano-particle modified paper substrate.
Application of the paper substrate of metal oxide nanoparticles modification of the present invention in sample detection.
Application of the present invention, the prohibitive dye in toy for children sample, specific bag are detected using paper ESI-MSr
Include following steps：
The paper substrate that the metal oxide nanoparticles are modified cuts a triangle paper substrate, by the toy for children sample
Product are loaded on the triangle paper substrate, and the base of the triangle paper substrate is clamped with metal holder, the metal holder with it is outer
High voltage power supply connection is connect, the triangle paper substrate is disposed adjacent to the injection port position of mass detector；In the triangle paper substrate
Prohibitive dye component in upper dropwise addition extractant, application high pressure, the extractant extraction toy for children sample, and
The triangle paper substrate tip forms electron spray, and the mass detector obtains corresponding response signal.
Application of the present invention, wherein, the toy for children sample is wax crayon, watercolor pencil or tattoo sticker, using painting
Smear or inscription rubbing mode is loaded on the triangle scraps of paper.
Application of the present invention, wherein, a length of 0.5cm in triangle scraps of paper base, a height of 0.75cm, thickness is
0.34mm, drift angle is 30 °.
Application of the present invention, wherein, the extractant is dichloromethane:Methanol:Formic acid=80:20:1, ratio
For volume ratio, dripping quantity is 20 μ L；The high pressure is 3.2kV under positive ion mode.
Application of the present invention, wherein, the prohibitive dye is disperse blue 1, disperse blue 106, disperse orange 3, solvent yellow
1st, solvent yellow 2, alkalescence red 9, alkaline purple 1, disperse blue 124, disperse yellow 3, disperse orange 37, Red-1 200, solvent yellow 3 and alkalescence purple
3, totally 13 kinds.
Application of the present invention, wherein, the Mass Spectrometry Conditions of the mass detector are set to：
Capillary voltage：3.2kV；
Extraction voltage：3V；
Radio-frequency lens voltage：0.1V；
Ion source temperature：120℃；
Desolvation temperature：350℃；
Precursor ion, fragment ion, taper hole voltage, collision energy and the detection limit of 1 13 kinds of prohibitive dyes of table
Precursor ion, fragment ion, taper hole voltage, collision energy and the detection limit of 13 kinds of prohibitive dyes are shown in Table 1.
Metal oxide nanoparticles difference from prior art of the present invention is：
The paper substrate of metal oxide nanoparticles modification of the present invention is applied in the paper spray technique in sample detection field,
Without pretreatment, analyze speed is fast, cost is low, sensitivity is high, simple to operate, and the analysis of sample can be completed in 30 seconds, is passed through
Nano particle is modified to paper substrate, the response of target substance is remarkably improved.
The present invention is with the detection side for the paper substrate prohibitive dye in toy for children modified using metal oxide nanoparticles
Exemplified by application in method, it was confirmed that the advantage of product of the present invention.Meanwhile, the present invention establishes a kind of paper electrospray mass spectrometry rapid screening
The detection method of prohibitive dye in toy, method is easy, quick, and the field quick detection of toy for children can be achieved.
The present invention also has the following advantages that：
1st, present invention firstly provides Co3O4Nano-particle modified paper substrate, is played using paper ESI-MSr quick detection children
Has the banned substance in sample；
2nd, in application example, the present invention is suitable for using prohibitive dye in toy for children the detection of paper spray pattern
Quick detection, the detection limit of each dyestuff is located between 5-50 μ g/kg.
3rd, in application example, the invention enables the detected value of prohibitive dye in toy for children mass detector response
Value is improved, and improves about 5~10 times.Included dyestuff has alkaline purple 1, disperse blue 106, alkalescence red 9, disperse blue 1, disperse orange
3, solvent yellow 1, solvent yellow 2, disperse blue 124, disperse yellow 3, disperse orange 37, Red-1 200, solvent yellow 3, alkaline purple 3 etc..
Below in conjunction with the accompanying drawings to the present invention metal oxide nanoparticles modification paper substrate and its in sample detection
Using being described further.
Brief description of the drawings
Fig. 1 is Co in the present invention3O4The low enlargement ratio scanning electron microscope (SEM) photograph of nano particle；
Fig. 2 is Co in the present invention3O4Nano particle high magnification scanning electron microscope (SEM) photograph；
Fig. 3 is Co in the present invention3O4Nano particle transmission electron microscope picture；
Fig. 4 is Co in the present invention3O4Nano-particle modified paper substrate scanning electron microscope (SEM) photograph；
Fig. 5 is the mass spectrogram of the disperse blue 1 obtained using the method in the present invention；
Fig. 6 is the mass spectrogram of the disperse blue 106 obtained using the method in the present invention；
Fig. 7 is the mass spectrogram of the disperse orange 3 obtained using the method in the present invention；
Fig. 8 is the mass spectrogram of the solvent yellow 1 obtained using the method in the present invention；
Fig. 9 is the mass spectrogram of the solvent yellow 2 obtained using the method in the present invention；
Figure 10 is alkaline red 9 mass spectrogram obtained using the method in the present invention；
Figure 11 is the mass spectrogram of the alkaline purple 1 obtained using the method in the present invention；
Figure 12 is the mass spectrogram of the disperse blue 124 obtained using the method in the present invention；
Figure 13 is the mass spectrogram of the disperse yellow 3 obtained using the method in the present invention；
Figure 14 is the mass spectrogram of the disperse orange 37 obtained using the method in the present invention；
Figure 15 is the mass spectrogram of the Red-1 200 obtained using the method in the present invention；
Figure 16 is the mass spectrogram of the solvent yellow 3 obtained using the method in the present invention；
Figure 17 is the mass spectrogram of the alkaline purple 3 obtained using the method in the present invention；
Figure 18 is relative response of the different extractants to various dyestuffs in the present invention；
Figure 19 is relative response of the different solvents in the present invention to various dyestuff total amounts；
Figure 20 is relative response of the different proportion mixed solvent in the present invention to various dyestuffs；
Figure 21 is relative response of the different proportion mixed solvent in the present invention to various dyestuff total amounts；
Figure 22 is relative response of the different formic acid additions to various dyestuffs in the present invention；
Figure 23 is relative response of the different formic acid additions to various dyestuff total amounts in the present invention；
Figure 24 is relative response of the different chromatographic papers to various dyestuffs in the present invention；
Figure 25 is relative response of the different chromatographic papers to various dyestuff total amounts in the present invention；
Figure 26 is Co in the present invention3O4The relative response of various dyestuffs after nano-particle modified paper substrate；
Figure 27 is Co in the present invention3O4The relative response of various dyestuff total amounts after nano-particle modified paper substrate.
All English translators of Chinese occurred in Fig. 5~Figure 17 of the present invention are as follows：
m/z：Karyoplasmic ratio；
Relative abundance：Relative abundance.
Embodiment
Experiment reagent and instrument：
Waters Xevo TQ mass spectrographs；The reagents such as dichloromethane, methanol are chromatographically pure；Disperse orange 3 (purity 95%) and
Solvent yellow 3 (purity 99%) is purchased from Acros companies of the U.S.；Alkaline purple 1 (purity 84%), red 9 (purity 95%) of alkalescence, alkalescence purple
3 (purity 80%), disperse blue 124 (purity 70%) and solvent yellow 2 (purity 95%) are public purchased from Germany Dr.Ehrenstorfer
Department；Disperse blue 1 (purity 30%), solvent yellow 1 (purity 99%), disperse blue 106 (purity 95%), disperse yellow 3 (purity 30%),
Red-1 200 (purity 95%) and disperse orange 37 (purity 95%) are purchased from Sigma Co., USA.
Embodiment 1
A kind of preparation method of metal oxide nanoparticles (including preparation method and product, i.e. metal oxide nano
Particle)
Co3O4The preparation of nano particle is based on two step synthesis programs.Co is synthesized by hydro-thermal method first3(CO3)2(OH)6, so
Afterwards by synthesized Co3(CO3)2(OH)6Calcining, forms the porous nanostructured of layering.Concrete operations：It is by 25mL concentration
0.4M Co (CH3CO2)2·4H2O sample is added in the urea that 50mL concentration is 0.8M.After stirring 30 minutes, solution is turned
The stainless steel autoclave of teflon back boxing is moved on to, and is kept for 10 hours under 100 DEG C of constant temperature.By gained sediment deionization
Water washing three times, and dried 30 minutes at 60 DEG C.Finally, by from room temperature with 1 DEG C/min speed be warming up to 400 DEG C and
400 DEG C are kept for 80 minutes, and calcining obtains nano Co3O4Particle.
The Co obtained by ESEM and transmission electron microscope observing3O4Nano particle, low enlargement ratio scanning electron microscope (SEM) photograph (figure
1) Co is shown3O4Nano particle is made up of substantial amounts of wire nanostructured.The scanning electron microscope (SEM) photograph (Fig. 2) and transmission electron microscope picture of amplification
(Fig. 3) is shown, wire Co3O4Nanostructured is actually made up of many ultrathin nanometer particles (diameter about 10nm).
Embodiment 2
Co3O4The paper substrate of nano-particle modified paper substrate, i.e. metal oxide nanoparticles modification：
Take the Co prepared3O40.5~1g of particle, it is scattered with 30~50mL absolute ethyl alcohols after grinding 20~30 minutes,
And stir 10~20 minutes.Chromatographic paper is laid on flat polytetrafluoroethylene, there is uniform under this polytetrafluoroethylene
Space be used for filtering solution.By Co3O4Homogeneous dispersion is scattered on polytetrafluoroethylene, 8~10 is stood at room temperature small
When, treat that ethanol solution volatilizees completely.Obtain dry Co3O4Nano-particle modified paper substrate.Co3O4It is nano-particle modified
Paper substrate scanning electron microscope (SEM) photograph it is as shown in Figure 4.
Embodiment 3
Co3O4Nano-particle modified 3MM grades of chromatographic paper
Take the Co that the first step is obtained3O4Nano particle 0.5g, it is scattered with 30mL absolute ethyl alcohols after grinding 20 minutes, and stir
10 minutes.3MM grades of chromatographic papers are laid on flat polytetrafluoroethylene, there is uniform space under this polytetrafluoroethylene
For filtering solution.By Co3O4Homogeneous dispersion is scattered on polytetrafluoroethylene, is stood 8 hours at room temperature, is treated anhydrous second
Alcoholic solution volatilizees completely.Obtain Co3O4Nano-particle modified 3MM level chromatographic papers.
Embodiment 4
Co3O4Nano-particle modified 3MM grades of chromatographic paper
Take the Co prepared3O4Nano particle 1g, it is scattered with 50mL absolute ethyl alcohols after grinding 30 minutes, and stir 20 points
Clock.3MM grades of chromatographic papers are laid on flat polytetrafluoroethylene, have uniform space to be used under this polytetrafluoroethylene
Filtering solution.By Co3O4Homogeneous dispersion is scattered on polytetrafluoroethylene, is stood 10 hours at room temperature, is treated that absolute ethyl alcohol is molten
Liquid volatilizees completely.Obtain Co3O4Nano-particle modified 3MM level chromatographic papers.
Embodiment 5
Co3O4Nano-particle modified 3MM grades of chromatographic paper
Take the Co prepared3O4Nano particle 0.8g, it is scattered with 40mL ethanol after grinding 25 minutes, and stir 15 points
Clock.3MM grades of chromatographic papers are laid on flat polytetrafluoroethylene, have uniform space to be used under this polytetrafluoroethylene
Filtering solution.By Co3O4Homogeneous dispersion is scattered on polytetrafluoroethylene, is stood 9 hours at room temperature, is treated that ethanol solution is complete
Full volatilization.Obtain Co3O4The 3MM level chromatographic papers of modification.
Embodiment 6
Prohibitive dye in paper ESI-MSr quick detection toy for children：
By Co3O4Nano-particle modified chromatographic paper is cut into base for 0.5cm, and a height of 0.75cm, thickness is 0.34mm, top
Angle is 30 ° of triangle paper substrate.By modes such as toy for children sample (such as wax crayon, watercolor pencil or tattoo sticker) smearing or inscription rubbings
It is loaded on triangle paper substrate, triangle paper substrate base is clamped with metal holder, and is connected on external high voltage power supply.Extraction is added dropwise
Take solvent (dichloromethane:Methanol:Formic acid=80:20:1, volume ratio) 20 μ L, high pressure is 3.5kV under positive ion mode.In high pressure
Under effect, the prohibitive dye in extractant extraction toy for children sample, and form electron spray, Mass Spectrometer Method at chromatographic paper tip
Device obtains corresponding response signal.
The Mass Spectrometry Conditions of mass detector are set to：
Capillary voltage：3.2kV；
Extraction voltage：3V；
Radio-frequency lens voltage：0.1V；
Ion source temperature：120℃；
Desolvation temperature：350℃；
Precursor ion, fragment ion, taper hole voltage, collision energy and the detection limit of 1 13 kinds of prohibitive dyes of table
After testing, using Co3O4The chromatographic paper of nano-particle modified mistake is sprayed as paper, the substance responds value of 13 kinds of dyestuffs
Improve about 5~10 times.The test limit of each material is determined with about 3 times of signal to noise ratio, their detection limit is located between 5-50 μ g/kg.
As shown in table 1, their Information in Mass Spectra figure is as shown in Fig. 5~Figure 17 for 13 kinds of prohibitive dye material informations.
2 13 kinds of prohibitive dye material informations of table
Discuss：
1st, the optimization of extractant
1) selection of extractant, have selected opposed polarity and volatile solvent, including n-hexane, tetrahydrofuran, second
Acetoacetic ester, chloroform, dichloromethane, acetone, acetonitrile, isopropanol, first alcohol and water, investigate their shadows to various dyestuff effect of extracting
Ring, as a result as depicted in figs. 18-19.As can be known from the results, total extraction of the two kinds of extractants of dichloromethane and methanol to various dyestuffs
Preferably, therefore, selection dichloromethane and methanol are extractant to effect.
2) different proportion dichloromethane and methanol mixed solvent (100% dichloromethane, dichloro on this basis, are compared
Methane:Methanol=20:80, dichloromethane:Methanol=40:60, dichloromethane:Methanol=60:40, dichloromethane:Methanol=80:
20,100% methanol) to the extraction results of various dyestuffs, as a result as shown in figures 20-21.It can be seen that dichloromethane and methanol
According to 80:During 20 volume ratio, response highest.
3) determine dichloromethane and methanol according to 80:After 20 volume ratios, different proportion formic acid is added in mixed solution
(0.1%, 0.3%, 0.5%, 1%, 1.5%), to improve overall response value.As a result as shown in figs. 22-23.Understand, formic acid addition
Measure for 1% when, various dyestuff overall response value highests.Therefore, it is final to determine that extractant is dichloromethane:Methanol:Formic acid=80:
20:1 (volume ratio).
2nd, the optimization of chromatographic paper
It is determined that after optimal extractant, we have carried out selection optimization to paper substrate.1 grade, 17 grades, 31ET grades is selected respectively
Investigated with four kinds of chromatographic papers of 3MM levels, as a result as shown in figures 24-25.It can be seen that 3MM grades of chromatographic papers are optimal.
3rd, contrast test
By Co3O4Nano-particle modified to 3MM grades chromatographic papers, relatively more various dyestuff responses, as a result as shown in figs. 26-27.
It can be seen that the response of various dyestuffs has different degrees of raising.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, technical side of the those of ordinary skill in the art to the present invention
In various modifications and improvement that case is made, the protection domain that claims of the present invention determination all should be fallen into.
Claims (10)
1. a kind of preparation method of metal oxide nanoparticles, it is characterised in that：Comprise the following steps：
By the Co (CH that 25mL concentration is 0.4M3CO2)2·4H2O sample is added in the urea that 50mL concentration is 0.8M, stirring 30
After minute, in the stainless steel autoclave for transferring the solution into teflon back boxing, and placed 10 hours under 100 DEG C of constant temperatures；
Resulting sediment is washed with deionized three times, and dried 30 minutes at 60 DEG C；Finally, by from room temperature with 1 DEG C/
Min speed is warming up to 400 DEG C and kept for 80 minutes under the conditions of 400 DEG C, and calcining obtains Co3O4Nano particle.
2. a kind of paper substrate of metal oxide nanoparticles modification, it is characterised in that：Including the Co described in claim 13O4Nanometer
Particle.
3. the preparation method of the paper substrate of the metal oxide nanoparticles modification described in claim 2, it is characterised in that：Including such as
Lower step：
Weigh the obtained Co3O40.5~1g of nano particle, after grinding 20~30 minutes, with 30~50mL absolute ethyl alcohols point
Dissipate, and stir 10~20 minutes, obtain Co3O4Dispersion liquid, chromatographic paper is laid on flat polytetrafluoroethylene, described
There is uniform space to be used for filtering solution under polytetrafluoroethylene, by the Co3O4Homogeneous dispersion is scattered in the polytetrafluoro
On ethene flat board, 8~10 hours are stood at room temperature, treats that ethanol solution volatilizees completely, obtains dry metal oxide and receive
The paper substrate of rice grain modification.
4. application of the paper substrate of the metal oxide nanoparticles modification described in claim 2 in sample detection.
5. application according to claim 4, it is characterised in that：Using in paper ESI-MSr detection toy for children sample
Prohibitive dye, specifically includes following steps：
The paper substrate that the metal oxide nanoparticles are modified cuts a triangle paper substrate, and the toy for children sample is added
It is downloaded on the triangle paper substrate, the base of the triangle paper substrate is clamped with metal holder, the metal holder and external height
Voltage source is connected, and the triangle paper substrate is disposed adjacent to the injection port position of mass detector；Dripped on the triangle paper substrate
Plus extractant, apply high pressure, the extractant extracts the prohibitive dye component in the toy for children sample, and described
Triangle paper substrate tip forms electron spray, and the mass detector obtains corresponding response signal.
6. application according to claim 5, it is characterised in that：The toy for children sample is wax crayon, watercolor pencil or tatooed
Paster, is loaded on the triangle paper substrate using smearing or inscription rubbing mode.
7. application according to claim 6, it is characterised in that：The triangle paper substrate bottom side length is 0.5cm, a height of
0.75cm, thickness is 0.34mm, and drift angle is 30 °.
8. application according to claim 7, it is characterised in that：The extractant is dichloromethane:Methanol:Formic acid=
80:20:1, ratio is volume ratio, and dripping quantity is 20 μ L；The high pressure is 3.2kV under positive ion mode.
9. application according to claim 8, it is characterised in that：The prohibitive dye is disperse blue 1, disperse blue 106, disperseed
Orange 3, solvent yellow 1, solvent yellow 2, alkalescence red 9, alkaline purple 1, disperse blue 124, disperse yellow 3, disperse orange 37, Red-1 200, solvent yellow
3 and alkaline purple 3, totally 13 kinds.
10. application according to claim 9, it is characterised in that：The Mass Spectrometry Conditions of the mass detector are set to：
Capillary voltage：3.2kV；
Extraction voltage：3V；
Radio-frequency lens voltage：0.1V；
Ion source temperature：120℃；
Desolvation temperature：350℃；
Precursor ion, fragment ion, taper hole voltage, collision energy and the detection limit of 1 13 kinds of prohibitive dyes of table
Precursor ion, fragment ion, taper hole voltage, collision energy and the detection limit of 13 kinds of prohibitive dyes are shown in Table 1.
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| CN109187713A (en) * | 2018-10-17 | 2019-01-11 | 湖南师范大学 | Load paper base, preparation method and ion source and its application |
| CN111239238A (en) * | 2020-02-03 | 2020-06-05 | 华南农业大学 | Rapid mass spectrometry imaging method for tissue sample |
| CN112958055A (en) * | 2021-01-29 | 2021-06-15 | 山东师范大学 | Adsorbing material for water pollutants, preparation method and mass spectrum detection application thereof |
| CN112958055B (en) * | 2021-01-29 | 2022-09-09 | 山东师范大学 | Adsorbing material for water pollutants, preparation method and mass spectrum detection application thereof |
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