CN113018908A - Preparation method of solid-phase micro-extraction device with velvet carbon nitride as coating - Google Patents
Preparation method of solid-phase micro-extraction device with velvet carbon nitride as coating Download PDFInfo
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Abstract
The invention discloses a preparation method of a solid phase micro-extraction device taking velvet carbon nitride as a coating, which can be applied to extraction of trace polycyclic aromatic hydrocarbon in environment and food and comprises the following steps: (1) pretreating a stainless steel wire; (2) preparing velvet carbon nitride and sol-gel solution mixed with the velvet carbon nitride; (3) preparing a solid phase microextraction coating; (4) and (5) assembling the solid phase micro-extraction device. The method is simple, raw materials are easy to obtain, the prepared coating is uniform in distribution, high-temperature resistant and not easy to fall off, the coating is easy to assemble and disassemble on a self-made extraction device, rapid extraction of polycyclic aromatic hydrocarbon can be realized, the thickness of the coating can be effectively regulated and controlled through repeated coating, and the enrichment capacity of the extraction device is ensured.
Description
Technical Field
The invention belongs to the technical field of sample pretreatment, and particularly relates to a preparation method of a solid phase micro-extraction device with velvet carbon nitride as a coating.
Background
Polycyclic aromatic hydrocarbons are harmful substances generated by fuels such as petroleum and coal, and wood and combustible gas under incomplete combustion or high-temperature treatment conditions, refer to aromatic hydrocarbons containing two or more benzene rings, and can cause various damages to human bodies, such as damages to respiratory systems, circulating systems, nervous systems and the like. Therefore, polycyclic aromatic hydrocarbons are identified as major organic pollutants affecting human health. Polycyclic aromatic hydrocarbons are usually present in trace amounts in the environment, food, and require pretreatment of the sample before measurement by gas chromatography.
The solid phase micro-extraction has the advantages of simple operation, no need of extraction solvent, on-line or living body sampling, automation, direct desorption in an analysis system and the like, and the technology has good application prospect in the fields of food, medicine, clinic and the like. For solid phase microextraction technology, the preparation of extraction coatings is the most important factor affecting its extraction capacity. The velvet carbon nitride is prepared by taking urea as a raw material and controlling the heating condition. Compared with carbon nitride material obtained by taking melamine as a precursor, the material has larger specific surface area, and the material is easier to peel off into a single layer and has more binding sites with a target object under ultrasonic treatment.
Based on this, the experimental selection velvet-shaped carbon nitride is used as the solid phase micro-extraction coating, compared with the carbon nitride coating obtained by the traditional preparation method, the specific surface area is larger, the extraction efficiency is higher, and the detection limit of the method on polycyclic aromatic hydrocarbon reaches 0.02-0.03 mu g/L.
Disclosure of Invention
The invention provides a preparation method of a solid phase micro-extraction device taking velvet carbon nitride as a coating, and the extraction device can be used for extracting polycyclic aromatic hydrocarbon in a sample. The purpose of the invention is realized by the following technical scheme:
a preparation method of a solid phase micro-extraction device taking velvet carbon nitride as a coating comprises the following steps:
(1) pretreating the stainless steel wire:
immersing the stainless steel wire into HF for corrosion treatment, washing the stainless steel wire with deionized water, and then drying the stainless steel wire at room temperature for 24 hours for later use;
(2) preparing a sol-gel solution of velvet carbon nitride and the velvet carbon nitride mixed sol-gel solution:
dissolving urea in water, transferring to a crucible after urea is completely dissolved, and placing in a sealed environmentThe velvet carbon nitride V-g-C is obtained under the condition of medium temperature control heating3N4(ii) a Mixing the velvet carbon nitride, dichloromethane, hydroxy polydimethylsiloxane and methyl trimethoxy silane uniformly by vortex, adding trifluoroacetic acid (95% aqueous solution) into the mixture, and performing vortex for a certain time to obtain a sol-gel solution mixed with the velvet carbon nitride;
(3) preparing a solid-phase microextraction coating:
immersing the pretreated stainless steel wire into a sol-gel solution mixed with velvet carbon nitride for soaking for a certain time, drying at room temperature, immersing again, and repeating the steps to form a sol-gel coating mixed with the velvet carbon nitride on the surface of the stainless steel wire;
(4) assembling a solid phase micro-extraction device:
and (4) drying the sol-gel coating mixed with the velvet carbon nitride prepared in the step (3) at room temperature, then putting the sol-gel coating into a solid phase micro-extraction device to obtain the extraction enrichment device, and carrying out aging treatment under the protection of nitrogen before use.
Further, in the step (2), the preparation of the sol-gel solution mixed with the velvet carbon nitride is that the velvet carbon nitride: dichloromethane: hydroxy polydimethylsiloxane: methyltrimethoxysilane: trifluoroacetic acid (95% aqueous solution) =30-50 mg: 100-: 100-: 100-: 60-80 μ L, preferably in a ratio of 30 mg: 100 μ L of: 200 μ L: 100 μ L of: 70 μ L.
Further, the coating in the step (3) is repeated 4 to 10 times, preferably 8 times.
Further, the step (4) is aged for 2-6h, preferably 4h at 280 ℃ under the protection of nitrogen before use.
The solid phase micro-extraction device with the velvet carbon nitride as the coating, which is prepared by the invention, is used for extracting polycyclic aromatic hydrocarbons in biscuits, has high extraction efficiency and low detection limit, and can realize sensitive detection of polycyclic aromatic hydrocarbons in complex samples.
FIG. 1 is a diagram of a self-made solid phase micro-extraction device, which is obtained by modifying a 5 μ L micro-sampler, wherein a stainless steel wire is fixed on a push rod, and the needle head part is coated with a 5cm stainless steel needle (22G needle head, high temperature resistant over 300 ℃).
FIG. 2 is a SEM image showing the surface roughness of a stainless steel wire treated with HF, and the surface of the coated fiber is coated with a sol-gel coating mixed with velvet carbon nitride.
FIG. 3 is a FT-IR chart of a velvet-like carbon nitride coating, in which 800 cm is shown in a spectrum-1 The ring plane of the triazine unit is located at a bending vibration absorption peak of 3000-3500 cm-1Is a characteristic peak of N-H stretching vibration, 1200-1700 cm-1The absorption bands in between are characteristic absorption peaks belonging to the heterocyclic compounds C-N and C = N, demonstrating successful modification of carbon nitride.
Fig. 8 is an SEM image of the same number of times and the same concentration of the velvet-like carbon nitride prepared by the present invention and the carbon nitride prepared by directly heating melamine in a muffle furnace, the left side is the carbon nitride prepared by directly heating melamine in the muffle furnace, and the right side is the velvet-like carbon nitride prepared by the present invention, and it is apparent from fig. 8 that the velvet-like carbon nitride prepared by the present invention is velvet-like and has a larger specific surface area.
Compared with the prior art, the invention has the beneficial effects that:
(1) the coating provided by the invention has the main component of velvet carbon nitride, and compared with a coating taking carbon nitride as a main component, the coating has the advantages of larger specific surface area, better extraction effect on polycyclic aromatic hydrocarbon, simple preparation compared with a commercial coating, easily obtained raw materials, high temperature resistance and difficulty in falling off;
(2) compared with the common quartz fiber used in solid phase micro-extraction, the stainless steel wire used as the support material has the advantages of high mechanical strength, long service life and easy assembly and disassembly on a self-made solid phase micro-extraction device;
(3) compared with physical methods, electrochemical deposition methods, chemical bonding methods and molecular imprinting methods, the sol-gel technology is simple and convenient, the prepared coating is firmer, and the thickness of the coating can be regulated and controlled by a repeated coating method.
Drawings
FIG. 1 is a diagram of a self-made solid phase micro-extraction device.
Fig. 2 is an SEM image of the velvet-like carbon nitride coating described in example 1.
FIG. 3 is a FT-IR plot of the velvet-like carbon nitride coating described in example 1.
FIG. 4 is a gas phase detection diagram of polycyclic aromatic hydrocarbon enrichment of the solid phase micro-extraction apparatus of example 2.
Fig. 5 is an optimization of the preparation method of velvet carbon nitride coating (polycyclic aromatic hydrocarbon enrichment) in example 3.
FIG. 6 is a graph of the spiked extract of polycyclic aromatic hydrocarbons in actual sample biscuits from the velvet carbon nitride coating of example 4.
FIG. 7 is a gas phase detection graph of polycyclic aromatic hydrocarbon enrichment in a solid phase micro-extraction apparatus using different coatings in a comparative example.
Fig. 8 is an SEM image of velvet-like carbon nitride prepared by the present invention in the comparative example at the same times as carbon nitride prepared by directly heating melamine in a muffle furnace.
Detailed Description
Example 1
(1) Pretreating the stainless steel wire:
immersing a stainless steel wire with the diameter of 0.3mm and the length of 20cm into HF for corrosion treatment for 30min, then washing the stainless steel wire clean with deionized water, and then drying the stainless steel wire for 24h at room temperature for later use;
(2) preparing a sol-gel solution of velvet carbon nitride and the velvet carbon nitride mixed sol-gel solution:
dissolving 15g of urea in 20mL of water, transferring the urea into a crucible after the urea is completely dissolved, and heating at a controlled temperature in a closed environment (400 ℃ for 1h and 450 ℃ for 2h) to obtain velvet-shaped carbon nitride V-g-C3N4(ii) a Vortex mixing the velvet carbon nitride (30mg) with dichloromethane (100 μ L), hydroxy polydimethylsiloxane (200 μ L) and methyltrimethoxysilane (100 μ L) for 5min, adding trifluoroacetic acid (70 μ L), and vortex for 2min to obtain sol-gel solution mixed with velvet carbon nitride;
(3) preparing a solid-phase microextraction coating:
immersing the pretreated stainless steel wire into a sol-gel solution mixed with the velvet carbon nitride for 2min, drying at room temperature, immersing again, repeating the operation for 8 times, and forming a sol-gel coating mixed with the velvet carbon nitride on the surface of the stainless steel wire;
(4) assembling a solid phase micro-extraction device:
the stainless steel wire coated with the sol-gel coating mixed with the velvet carbon nitride is dried at room temperature for 24 hours, then is put into a solid phase micro-extraction device, and is aged for 4 hours at 280 ℃ under the protection of nitrogen before use.
Example 2
The solid phase micro-extraction device which is prepared by the invention and takes the velvet carbon nitride as the coating is used for extracting the polycyclic aromatic hydrocarbon in the sample, and the polycyclic aromatic hydrocarbon in the sample solution is extracted by adopting a direct immersion extraction mode, and the specific operation is as follows:
putting a brown small bottle filled with 20mL of sample solution (the adding concentration of five polycyclic aromatic hydrocarbons, namely acenaphthene, fluorene, anthracene, fluoranthene and pyrene is 100 mug/L) into a constant-temperature heating magnetic stirring water bath kettle, then inserting the prepared solid phase micro-extraction device into the bottle, pushing out a stainless steel wire, completely inserting the coating part into the sample solution, adjusting the temperature of the constant-temperature heating magnetic stirring water bath kettle to 35 ℃, adjusting the rotating speed to 50rpm, stirring for 30min, and finishing extraction. The solid phase micro-extraction device is inserted into a gas chromatography sample inlet, and is thermally desorbed for 5min at 280 ℃ under the assistance of nitrogen, and quantitative analysis is carried out through gas chromatography. The results of the detection are shown in FIG. 4.
Example 3
In order to examine the effect of the amount of velvet carbon nitride added on the extraction effect, the same polycyclic aromatic hydrocarbon as that of example 2 was selected as the target, and V-g-C was changed under the same conditions as those of example 1 (except for the amount of velvet carbon nitride)3N4(0-50mg) in the amount of the following, several different velvet-like carbon nitride solid-phase microextraction coatings were prepared, then the extraction of example 2 was performed, and finally the results are shown in FIG. 5 by comparing the peak area analysis of the gas chromatogram, and it can be seen that as V-g-C is followed3N4The mass increase and extraction effect are also increasing, but when it is more than 30mg, the extraction effect begins to decrease, probably because too much velvet carbon nitride begins to accumulate and is not well dispersed, and the contact area with polycyclic aromatic hydrocarbon becomes small, resulting in thatThe extraction effect is reduced.
Example 4
In order to examine the extraction effect of the solid-phase micro-extraction device with the coating of the velvet-shaped carbon nitride prepared by the invention on actual samples, four kinds of biscuits purchased from a supermarket are selected as the actual samples, 1.0g of mashed biscuits are weighed on an analytical balance and transferred into a centrifuge tube, 5mL of acetone is added, vortex is carried out for 1min, and then ultrasonic extraction is carried out for 20min so as to fully mix the samples with the acetone. Centrifuging at 8000rpm for 5min, collecting supernatant, repeating the above extraction, mixing the two supernatants, and recovering N2After blowing, the sample is re-dissolved in 500 mul of acetone to obtain the actual sample solution. And (3) taking a sample bottle with a hole cover and a polytetrafluoroethylene spacer at the top end, cleaning and drying, adding five kinds of mixture standard samples of the polycyclic aromatic hydrocarbon into the actual sample solution to enable the adding standard concentration to be 25 microgram/L, immediately screwing the bottle cover, and uniformly mixing for extraction. FIG. 6 is a labeled extraction diagram of an actual sample of the biscuit extracted by the invention, and it can be seen that the solid phase micro-extraction device with the coating of velvet carbon nitride prepared by the invention can extract polycyclic aromatic hydrocarbons in the biscuit.
Comparative example
In order to prove that the coating prepared by the method has excellent extraction effect, the same polycyclic aromatic hydrocarbon is selected as a target object, and the extraction effect is compared with that of carbon nitride (shown in figure 8) prepared by directly heating melamine in a muffle furnace and that of an extraction target object when commercial PDMS is used as the coating, and the result is shown in figure 7, and the drawing proves that the extraction efficiency of the coating prepared by the method is 2 times that of the carbon nitride prepared by directly heating melamine in the muffle furnace and is 5-10 times that of the carbon nitride prepared by directly heating melamine in the muffle furnace and the commercial PDMS is used as the coating, so that the coating prepared by the method has excellent extraction effect on the polycyclic aromatic hydrocarbon in the biscuit.
Claims (10)
1. A preparation method of a solid phase micro-extraction device taking velvet carbon nitride as a coating is characterized by comprising the following steps:
(1) pretreating the stainless steel wire:
immersing the stainless steel wire into HF for corrosion treatment, washing the stainless steel wire with deionized water, and then drying the stainless steel wire at room temperature for 24 hours for later use;
(2) preparing a sol-gel solution of velvet carbon nitride and the velvet carbon nitride mixed sol-gel solution:
dissolving urea in water, transferring into crucible after urea is completely dissolved, and heating under controlled temperature in sealed environment to obtain velvet carbon nitride V-g-C3N4(ii) a Mixing the velvet carbon nitride, dichloromethane, hydroxy polydimethylsiloxane and methyl trimethoxy silane uniformly by vortex, adding trifluoroacetic acid (95% aqueous solution) into the mixture, and performing vortex for a certain time to obtain a sol-gel solution mixed with the velvet carbon nitride;
(3) preparing a solid-phase microextraction coating:
immersing the pretreated stainless steel wire into a sol-gel solution mixed with velvet carbon nitride for soaking for a certain time, drying at room temperature, immersing again, and repeating the steps to form a sol-gel coating mixed with the velvet carbon nitride on the surface of the stainless steel wire;
(4) assembling a solid phase micro-extraction device:
and (4) drying the sol-gel coating mixed with the velvet carbon nitride prepared in the step (3) at room temperature, then putting the sol-gel coating into a solid phase micro-extraction device to obtain the extraction enrichment device, and carrying out aging treatment under the protection of nitrogen before use.
2. The process (1) according to claim 1, wherein the stainless steel wire has a diameter of 0.3mm and a length of 20 cm.
3. The method according to claim 1 or 2, wherein the stainless steel wire is pretreated at one end thereof to have a length of 2 cm, subjected to HF etching for 30min, and dried at room temperature for 24 hours.
4. The step (2) of preparing the velvet-like carbon nitride according to claim 1, wherein the mass ratio of urea to water is 3: 4, keeping the temperature of 400 ℃ for 1h and keeping the temperature of 450 ℃ for 2 h.
5. The method for preparing a sol-gel solution mixed with velvet carbon nitride according to the step (2) of claim 1, wherein the weight ratio of velvet carbon nitride: dichloromethane: hydroxy polydimethylsiloxane: methyltrimethoxysilane: trifluoroacetic acid (95% aqueous solution) =30-50 mg: 100-: 100-: 100-: 60-80 μ L.
6. The method of preparing the sol-gel solution mixed with velvet carbon nitride according to step (2) of claim 1 or 5, wherein velvet carbon nitride, methylene chloride, hydroxy polydimethylsiloxane and methyltrimethoxysilane are added to a microcentrifuge tube and mixed by vortexing for 5min and after trifluoroacetic acid is added, vortexing for 2 min.
7. The method according to claim 1 to 6, wherein the stainless steel wire treated in the step (1) is dipped in the sol solution mixed with the velvet-like carbon nitride in the step (2) for 2min, and the coating is repeated 4 to 10 times.
8. The stainless steel wire coated in the step (4) according to claim 1 is dried at room temperature for 24h, and is aged at 280 ℃ for 2-6h under the protection of nitrogen before use.
9. The solid phase micro-extraction device of step (4) according to claim 1 or 8, which is obtained by modifying a micro-sampler using a 5cm stainless steel needle-protection coated stainless steel wire.
10. The method for preparing a solid phase micro-extraction device with velvet carbon nitride as a coating according to claims 1-9, wherein stainless steel wires are used as a support material, and sol-gel mixed with velvet carbon nitride is used as a coating material.
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| CN114984619A (en) * | 2022-04-20 | 2022-09-02 | 吉林化工学院 | Preparation method of solid phase micro-extraction device with oxygen-doped carbon nitride as coating |
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Application publication date: 20210625 |