CN104841406A - Dimethylaminopropyl imidazole-bonded filter paper solid-phase microextraction membrane and preparation method and application thereof - Google Patents
Dimethylaminopropyl imidazole-bonded filter paper solid-phase microextraction membrane and preparation method and application thereof Download PDFInfo
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- CN104841406A CN104841406A CN201510260146.4A CN201510260146A CN104841406A CN 104841406 A CN104841406 A CN 104841406A CN 201510260146 A CN201510260146 A CN 201510260146A CN 104841406 A CN104841406 A CN 104841406A
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Abstract
The invention discloses a dimethylaminopropyl imidazole-bonded filter paper solid-phase microextraction membrane and a preparation method and application thereof, which belong to the technical field of the enrichment analysis of vegetable oil. The key point of the technical solution of the invention is that N,N-dimethylaminopropyl imidazole is bonded onto a piece of filter paper by 3-chloropropyldiethoxy silane coupling agent, so that the dimethylaminopropyl imidazole-bonded filter paper solid-phase microextraction membrane is obtained. The invention also discloses the preparation method of the dimethylaminopropyl imidazole-bonded filter paper solid-phase microextraction membrane and the application of the dimethylaminopropyl imidazole-bonded filter paper solid-phase microextraction membrane in the enrichment analysis of phenolic substances in vegetable oil. By utilizing the characteristics of high stability and designability existing in ionic liquid, the invention bonds N,N-dimethylaminopropyl imidazole onto the filter paper by means of 3-chloropropyldiethoxy silane coupling agent, so that the paper-based solid-phase microextraction membrane is obtained, and the prepared solid-phase microextraction membrane has the advantages of easiness in preparation, convenience in operation and carrying, low cost, high stability, excellent extraction performance and the like.
Description
Technical field
The invention belongs to the enrichment analysis technical field of vegetable oil, be specifically related to a kind of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane and its preparation method and application.
Background technology
SPME a kind ofly integrates sampling, purification, is separated and the Sample Pretreatment Technique of enrichment, has easy and simple to handle, quick, sample and solvent load is few, extraction efficiency is high and be easy to the advantages such as control automatically.But solid phase micro-extraction extraction head has the shortcomings such as high, the frangible and poor reproducibility of price, research and development novel solid phase micro extraction material is important study hotspot.
Summary of the invention
The technical problem that the present invention solves there is provided and is a kind ofly easy to preparation, convenient operation and carrying and dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane with low cost and preparation method thereof, and obtained dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane can be used in the enrichment analysis of aldehydes matter in vegetable oil.
The present invention adopts following technical scheme for solving the problems of the technologies described above, a kind of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane, it is characterized in that by 3-chloropropyl diethoxy silane coupling agent N, N-dimethyl aminopropyl imidazoles being bonded on filter paper forming dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane.
The preparation method of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane of the present invention, it is characterized in that comprising the following steps: (1) acetone washs filter paper and room temperature is dried for subsequent use, with 19mL absolute ethyl alcohol for solvent, 4.7g N, N-dimethyl aminopropyl imidazoles and 6.02g 3-chloropropyl triethoxysilane are obtained product A in 80 DEG C of reaction 24h for subsequent use; (2) 12g product A being joined volume ratio is form mixed system in the absolute ethyl alcohol of 1:4 and the mixed solvent of toluene, get the above-mentioned filter paper that dries and squirt with the distilled water with quality such as filter paper, then join in above-mentioned mixed system in 105 DEG C of reaction 24h, the filter paper obtained is first the mixed solution washing of the toluene of 4:1 and ethanol by volume ratio, use absolute ethanol washing again, then obtain dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane in 60 DEG C of dryings.
Dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane of the present invention analyzes the application of aldehydes matter in vegetable oil in enrichment, it is characterized in that concrete grammar is: the drafting of (1) calibration curve, in a series of conical flask, add the mixed solution of 1mL fresh plant oil, the paranitrophenol of 200 μ L different quality concentration gradients and 2,4-dinitrophenol dinitrophenolate, 9mL n-hexane and 5 μ L molar concentrations is respectively 2mol L
-1sodium hydroxide solution, the dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane again size being respectively 1cm*2cm to add in conical flask and seals, then 70min are adsorbed with the rotating speed of 160r/min in 30 DEG C of vibrations, take out the washing of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane, dry rear use 1100 μ L eluent 10min, wherein eluant, eluent is volume ratio is the acetonitrile of 50:1 and the mixed solution of concentrated hydrochloric acid, nitrogen dries up the chromatographically pure methyl alcohol of rear use 50 μ L and dissolves, and the parameter of setting liquid chromatograph is respectively C
18post 4.6mm × 250mm, column temperature 25 DEG C, mobile phase is the water of volume ratio 42:58 and the mixed solution of methyl alcohol, and wherein containing mass concentration in water is the acetic acid of 1%, and containing mass concentration in methyl alcohol is the acetic acid of 1%, flow velocity 1mL min
-1, determined wavelength is 230nm, Drawing of Curve concentration-peak area calibration curve that concentration and liquid chromatograph according to preparation sample obtain; (2) the enrichment analysis of testing sample, in conical flask, add 1mL vegetable oil to be measured, 9mL n-hexane and 5 μ L molar concentrations is 2mol L
-1sodium hydroxide solution, again the dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane being of a size of 1cm*2cm to be added in conical flask and to seal, then 70min are adsorbed with the rotating speed of 160r/min in 30 DEG C of vibrations, take out the washing of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane, dry rear use 1100 μ L eluent 10min, wherein eluant, eluent is volume ratio is the acetonitrile of 50:1 and the mixed solution of concentrated hydrochloric acid, nitrogen dries up the chromatographically pure methyl alcohol of rear use 50 μ L and dissolves, and the parameter of setting liquid chromatograph is respectively C
18post 4.6mm × 250mm, column temperature 25 DEG C, mobile phase is the water of volume ratio 42:58 and the mixed solution of methyl alcohol, and wherein containing mass concentration in water is the acetic acid of 1%, and containing mass concentration in methyl alcohol is the acetic acid of 1%, flow velocity 1mL min
-1, determined wavelength is 230nm, calculates peak area according to the curve that liquid chromatograph obtains and calculates the concentration of paranitrophenol and 2,4-dinitrophenol dinitrophenolate in vegetable oil to be measured according to concentration-peak area calibration curve.
The present invention utilizes ionic liquid good stability and programmable feature, by 3-chloropropyl triethoxysilane coupling agent by N, N-dimethyl aminopropyl imidazoles is bonded on filter paper and forms paper substrate solid-phase extraction membrane, because filter paper is cheap and easy to get, frivolous, flammable, biodegradable, be easy to transport, storage and recycling, easy cutting, the advantages such as easy processing, the solid-phase extraction membrane of preparation is had be easy to preparation, convenient operation and carry, with low cost, good stability and the advantage such as extraction ability is excellent.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane that the embodiment of the present invention 1 obtains, Fig. 2 is the scanning electron microscope (SEM) photograph of filter paper, and Fig. 3 is the scanning electron microscope (SEM) photograph of the dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane that the embodiment of the present invention 1 obtains.
Detailed description of the invention
Be described in further details foregoing of the present invention by the following examples, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
The preparation of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane
(1) acetone washing filter paper room temperature is dried for subsequent use, with 19mL absolute ethyl alcohol for solvent, obtains product A by 4.7g N, N-dimethyl aminopropyl imidazoles and 6.02g 3-chloropropyl triethoxysilane in 80 DEG C of reaction 24h for subsequent use;
(2) 12g product A being added to volume ratio is form mixed system in the absolute ethyl alcohol of 1:4 and the mixed solvent of toluene, get the filter paper after drying and squirt with the distilled water with quality such as filter paper, then join in above-mentioned mixed system in 105 DEG C of reaction 24h, the filter paper obtained is first the mixed solution washing of the toluene of 4:1 and ethanol by volume ratio, use absolute ethanol washing again, then obtain dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane in 60 DEG C of dryings.
Embodiment 2
(1) drafting of calibration curve, in a series of conical flask, add the mixed solution of 1mL fresh plant oil, the paranitrophenol of 200 μ L different quality concentration gradients and 2,4-dinitrophenol dinitrophenolate, 9mL n-hexane and 5 μ L molar concentrations is respectively 2mol L
-1sodium hydroxide solution, the dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane again size being respectively 1cm*2cm to add in conical flask and seals, then 70min are adsorbed with the rotating speed of 160r/min in 30 DEG C of vibrations, take out the washing of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane, dry rear use 1100 μ L eluent 10min, wherein eluant, eluent is volume ratio is the acetonitrile of 50:1 and the mixed solution of concentrated hydrochloric acid, nitrogen dries up the chromatographically pure methyl alcohol of rear use 50 μ L and dissolves, and the parameter of setting liquid chromatograph is respectively C
18post 4.6mm × 250mm, column temperature 25 DEG C, mobile phase is the water of volume ratio 42:58 and the mixed solution of methyl alcohol, and wherein containing mass concentration in water is the acetic acid of 1%, and containing mass concentration in methyl alcohol is the acetic acid of 1%, flow velocity 1mL min
-1, determined wavelength is 230nm, Drawing of Curve concentration-peak area calibration curve that concentration and liquid chromatograph according to preparation sample obtain;
(2) the enrichment analysis of testing sample, in conical flask, add 1mL vegetable oil to be measured, 9mL n-hexane and 5 μ L molar concentrations is 2mol L
-1sodium hydroxide solution, again the dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane being of a size of 1cm*2cm to be added in conical flask and to seal, then 70min are adsorbed with the rotating speed of 160r/min in 30 DEG C of vibrations, take out the washing of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane, dry rear use 1100 μ L eluent 10min, wherein eluant, eluent is volume ratio is the acetonitrile of 50:1 and the mixed solution of concentrated hydrochloric acid, nitrogen dries up the chromatographically pure methyl alcohol of rear use 50 μ L and dissolves, and the parameter of setting liquid chromatograph is respectively C
18post 4.6mm × 250mm, column temperature 25 DEG C, mobile phase is the water of volume ratio 42:58 and the mixed solution of methyl alcohol, and wherein containing mass concentration in water is the acetic acid of 1%, and containing mass concentration in methyl alcohol is the acetic acid of 1%, flow velocity 1mL min
-1, determined wavelength is 230nm, calculates peak area according to the curve that liquid chromatograph obtains and calculates the concentration of paranitrophenol and 2,4-dinitrophenol dinitrophenolate in vegetable oil to be measured according to concentration-peak area calibration curve.
According to the experimental technique determined and condition determination, analyze paranitrophenol and 2,4-dinitrophenol dinitrophenolate simultaneously, mass concentration in the scope of 10-1000 μ g/L, the linearly dependent coefficient (r of calibration curve
2) be respectively 0.9935 and 0.9909, mass concentration is to the paranitrophenol and 2 of 200 μ g/L, in the vegetable oil of 4-dinitrophenol dinitrophenolate, relative standard deviation is respectively 2.4% and 5.4%, and this solid-phase extraction membrane can be used in the enrichment analysis of paranitrophenol and 2,4-dinitrophenol dinitrophenolate in vegetable oil.
Embodiment above describes general principle of the present invention, principal character and advantage; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; under the scope not departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (3)
1. a dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane, it is characterized in that by 3-chloropropyl diethoxy silane coupling agent N, N-dimethyl aminopropyl imidazoles being bonded on filter paper forming dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane.
2. the preparation method of a dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane according to claim 1, it is characterized in that comprising the following steps: (1) acetone washs filter paper and room temperature is dried for subsequent use, with 19mL absolute ethyl alcohol for solvent, 4.7g N, N-dimethyl aminopropyl imidazoles and 6.02g 3-chloropropyl triethoxysilane are obtained product A in 80 DEG C of reaction 24h for subsequent use; (2) 12g product A being joined volume ratio is form mixed system in the absolute ethyl alcohol of 1:4 and the mixed solvent of toluene, get the above-mentioned filter paper that dries and squirt with the distilled water with quality such as filter paper, then join in above-mentioned mixed system in 105 DEG C of reaction 24h, the filter paper obtained is first the mixed solution washing of the toluene of 4:1 and ethanol by volume ratio, use absolute ethanol washing again, then obtain dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane in 60 DEG C of dryings.
3. dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane according to claim 1 analyzes the application of aldehydes matter in vegetable oil in enrichment, it is characterized in that concrete grammar is: the drafting of (1) calibration curve, in a series of conical flask, add the mixed solution of 1mL fresh plant oil, the paranitrophenol of 200 μ L different quality concentration gradients and 2,4-dinitrophenol dinitrophenolate, 9mL n-hexane and 5 μ L molar concentrations is respectively 2mol L
-1sodium hydroxide solution, the dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane again size being respectively 1cm*2cm to add in conical flask and seals, then 70min are adsorbed with the rotating speed of 160r/min in 30 DEG C of vibrations, take out the washing of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane, dry rear use 1100 μ L eluent 10min, wherein eluant, eluent is volume ratio is the acetonitrile of 50:1 and the mixed solution of concentrated hydrochloric acid, nitrogen dries up the chromatographically pure methyl alcohol of rear use 50 μ L and dissolves, and the parameter of setting liquid chromatograph is respectively C
18post 4.6mm × 250mm, column temperature 25 DEG C, mobile phase is the water of volume ratio 42:58 and the mixed solution of methyl alcohol, and wherein containing mass concentration in water is the acetic acid of 1%, and containing mass concentration in methyl alcohol is the acetic acid of 1%, flow velocity 1mL min
-1, determined wavelength is 230nm, Drawing of Curve concentration-peak area calibration curve that concentration and liquid chromatograph according to preparation sample obtain; (2) the enrichment analysis of testing sample, in conical flask, add 1mL vegetable oil to be measured, 9mL n-hexane and 5 μ L molar concentrations is 2mol L
-1sodium hydroxide solution, again the dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane being of a size of 1cm*2cm to be added in conical flask and to seal, then 70min are adsorbed with the rotating speed of 160r/min in 30 DEG C of vibrations, take out the washing of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane, dry rear use 1100 μ L eluent 10min, wherein eluant, eluent is volume ratio is the acetonitrile of 50:1 and the mixed solution of concentrated hydrochloric acid, nitrogen dries up the chromatographically pure methyl alcohol of rear use 50 μ L and dissolves, and the parameter of setting liquid chromatograph is respectively C
18post 4.6mm × 250mm, column temperature 25 DEG C, mobile phase is the water of volume ratio 42:58 and the mixed solution of methyl alcohol, and wherein containing mass concentration in water is the acetic acid of 1%, and containing mass concentration in methyl alcohol is the acetic acid of 1%, flow velocity 1mL min
-1, determined wavelength is 230nm, calculates peak area according to the curve that liquid chromatograph obtains and calculates the concentration of paranitrophenol and 2,4-dinitrophenol dinitrophenolate in vegetable oil to be measured according to concentration-peak area calibration curve.
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| CN104402729A (en) * | 2014-12-10 | 2015-03-11 | 河南师范大学 | Method for adsorbing 2,4-dinitrophenol by adopting silica-bonded dimethyl acrylic amino imidazole solid-phase extraction agent |
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| CN104402729A (en) * | 2014-12-10 | 2015-03-11 | 河南师范大学 | Method for adsorbing 2,4-dinitrophenol by adopting silica-bonded dimethyl acrylic amino imidazole solid-phase extraction agent |
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| 王香凤等: "硅烷修饰滤纸固相微萃取-室温磷光法测定水样中7,8-苯并喹啉", 《分析化学》 * |
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