CN104841406B - A kind of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane and its preparation method and application - Google Patents
A kind of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane and its preparation method and application Download PDFInfo
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- CN104841406B CN104841406B CN201510260146.4A CN201510260146A CN104841406B CN 104841406 B CN104841406 B CN 104841406B CN 201510260146 A CN201510260146 A CN 201510260146A CN 104841406 B CN104841406 B CN 104841406B
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Abstract
The invention discloses a kind of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane and its preparation method and application, belong to the enrichment analysis technical field of vegetable oil.Technical scheme main points are that N dimethyl aminopropyl imidazoles, which is bonded on filter paper, forms dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane by 3 chloropropyl diethoxy silane coupling agents by N.The application of aldehydes matter in vegetable oil is analyzed the invention also discloses the preparation method of dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane and its in enrichment.The present invention utilizes ionic liquid stability good and programmable feature, by 3 chloropropyl triethoxysilane coupling agents by N, N dimethyl aminopropyl imidazoles is bonded on filter paper formation paper substrate solid-phase extraction membrane, the solid-phase extraction membrane of preparation have the advantages that it is easily prepared, be easy to operate and carry, with low cost, stability is good and extraction ability is excellent.
Description
Technical field
The invention belongs to the enrichment analysis technical field of vegetable oil, and in particular to a kind of dimethyl aminopropyl imidazoles bonding filter
Paper solid-phase extraction membrane and its preparation method and application.
Background technology
SPME is a kind of Sample Pretreatment Technique for integrating sampling, purification, separation and enrichment, with operation
It is easy, the advantages of quick, sample and solvent load are few, extraction efficiency is high and is easy to automatically control.However, solid-phase micro extraction
Head has the shortcomings that price is high, frangible and poor reproducibility, and it is important study hotspot to research and develop novel solid phase micro extraction material.
The content of the invention
Present invention solves the technical problem that there is provided it is a kind of it is easily prepared, be easy to operate and carry and with low cost two
Methyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane and preparation method thereof, obtained dimethyl aminopropyl imidazoles is bonded filter paper
Solid-phase extraction membrane can be used in the enrichment analysis of aldehydes matter in vegetable oil.
The present invention adopts the following technical scheme that a kind of dimethyl aminopropyl imidazoles is bonded filter paper to solve above-mentioned technical problem
Solid-phase extraction membrane, it is characterised in that be by N, N- dimethyl aminopropyl imidazoles by 3- chloropropyl diethoxy silane coupling agents
It is bonded on filter paper and forms dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane.
Dimethyl aminopropyl imidazoles of the present invention is bonded the preparation method of filter paper solid-phase extraction membrane, it is characterised in that
Comprise the following steps：（1）Acetone washing filter paper and room temperature dry it is standby, using 19mL absolute ethyl alcohols as solvent, by 4.7g N, N- bis-
It is standby that methyl aminopropyl imidazoles and 6.02g 3- chloropropyl triethoxysilanes obtain product A in 80 DEG C of reaction 24h；（2）By 12g
It is 1 that product A, which is added to volume ratio,:4 absolute ethyl alcohol and the in the mixed solvent formation mixed system of toluene, take the above-mentioned filter dried
Paper is simultaneously squirted with the distilled water with the quality such as filter paper, is then added in above-mentioned mixed system and is reacted 24h in 105 DEG C, obtains
Filter paper is first 4 with volume ratio:The mixed solution washing of 1 toluene and ethanol, then washed with absolute ethyl alcohol, then in 60 DEG C of dryings
Obtain dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane.
Dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane of the present invention phenol in enrichment analysis vegetable oil
The application of class material, it is characterised in that specific method is：（1）The drafting of standard curve, is separately added into a series of conical flasks
1mL fresh plants oil, the mixed solution of the paranitrophenol of 200 μ L different quality concentration gradients and 2,4- dinitrophenol dinitrophenolates, 9mL just oneself
Alkane and 5 μ L molar concentrations are 2mol L-1Sodium hydroxide solution, then by size be respectively 1cm*2cm dimethyl aminopropyl miaow
Azoles bonding filter paper solid-phase extraction membrane is added in conical flask and sealed, and is then adsorbed with 160r/min rotating speed in 30 DEG C of vibrations
70min, takes out the bonding filter paper solid-phase extraction membrane washing of dimethyl aminopropyl imidazoles, with 1100 μ L eluents after drying
10min, wherein eluant, eluent are that volume ratio is 50:1 acetonitrile and the mixed solution of concentrated hydrochloric acid, with 50 μ L chromatographically pures after nitrogen drying
Methanol dissolving, setting liquid chromatograph parameter be respectively C18Post 4.6mm × 250mm, 25 DEG C of column temperature, mobile phase is volume ratio
42:Containing the acetic acid that mass concentration is 1% in 58 water and the mixed solution of methanol, its reclaimed water, it is containing mass concentration in methanol
1% acetic acid, flow velocity 1mL min-1, Detection wavelength is 230nm, the song obtained according to the concentration and liquid chromatograph for preparing sample
Line draws concentration-peak area standard curve；（2）The enrichment analysis of testing sample, added in conical flask 1mL vegetable oil to be measured,
9mL n-hexanes and 5 μ L molar concentrations are 2mol L-1Sodium hydroxide solution, then by size be 1cm*2cm dimethyl aminopropyl
Imidazoles bonding filter paper solid-phase extraction membrane is added in conical flask and sealed, and is then adsorbed with 160r/min rotating speed in 30 DEG C of vibrations
70min, takes out the bonding filter paper solid-phase extraction membrane washing of dimethyl aminopropyl imidazoles, with 1100 μ L eluents after drying
10min, wherein eluant, eluent are that volume ratio is 50:1 acetonitrile and the mixed solution of concentrated hydrochloric acid, with 50 μ L chromatographically pures after nitrogen drying
Methanol dissolving, setting liquid chromatograph parameter be respectively C18Post 4.6mm × 250mm, 25 DEG C of column temperature, mobile phase is volume ratio
42:Containing the acetic acid that mass concentration is 1% in 58 water and the mixed solution of methanol, its reclaimed water, it is containing mass concentration in methanol
1% acetic acid, flow velocity 1mL min-1, Detection wavelength is 230nm, and peak area and root are calculated according to the curve that liquid chromatograph is obtained
The concentration for obtaining paranitrophenol and 2,4- dinitrophenol dinitrophenolates in vegetable oil to be measured is calculated according to concentration-peak area standard curve.
The present invention utilizes ionic liquid stability good and programmable feature, passes through 3- chloropropyl triethoxysilanes even
Join agent by N, N- dimethyl aminopropyl imidazoles is bonded to formation paper substrate solid-phase extraction membrane on filter paper, because filter paper is cheap and easy to get,
It is frivolous, flammable, biodegradable, it is easy to transport, store and recycle, easily cut, the advantages of easy processing, make the solid phase of preparation
Extraction membrane have the advantages that it is easily prepared, be easy to operate and carry, with low cost, stability is good and extraction ability is excellent.
Brief description of the drawings
Fig. 1 is the infrared light that dimethyl aminopropyl imidazoles made from the embodiment of the present invention 1 is bonded filter paper solid-phase extraction membrane
Spectrogram, Fig. 2 is the scanning electron microscope (SEM) photograph of filter paper, and Fig. 3 is that dimethyl aminopropyl imidazoles bonding filter paper is consolidated made from the embodiment of the present invention 1
The scanning electron microscope (SEM) photograph of phase extraction film.
Embodiment
The above to the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
Dimethyl aminopropyl imidazoles is bonded the preparation of filter paper solid-phase extraction membrane
（1）Acetone washing filter paper and room temperature dry it is standby, using 19mL absolute ethyl alcohols as solvent, by 4.7g N, N- dimethyl
It is standby that aminopropyl imidazoles and 6.02g 3- chloropropyl triethoxysilanes obtain product A in 80 DEG C of reaction 24h；
（2）It is 1 that 12g products A is added into volume ratio:4 absolute ethyl alcohol and the in the mixed solvent formation mixed system of toluene,
Take the filter paper after drying and squirted with the distilled water with the quality such as filter paper, is then added in above-mentioned mixed system anti-in 105 DEG C
24h is answered, obtained filter paper is first 4 with volume ratio:The mixed solution washing of 1 toluene and ethanol, then washed with absolute ethyl alcohol, so
Dimethyl aminopropyl imidazoles bonding filter paper solid-phase extraction membrane is dried to obtain after 60 DEG C.
Embodiment 2
（1）The drafting of standard curve, is separately added into 1mL fresh plants oil, 200 μ L different qualities in a series of conical flasks
The paranitrophenol of concentration gradient and the mixed solution of 2,4- dinitrophenol dinitrophenolates, 9mL n-hexanes and 5 μ L molar concentrations are 2mol L-1's
Sodium hydroxide solution, then the dimethyl aminopropyl imidazoles that size is respectively 1cm*2cm is bonded the addition of filter paper solid-phase extraction membrane
In conical flask and seal, dimethyl aminopropyl imidazoles key is then taken out in 30 DEG C of vibration absorption 70min with 160r/min rotating speed
The washing of filter paper solid-phase extraction membrane is closed, with 1100 μ L eluent 10min after drying, wherein eluant, eluent is that volume ratio is 50:1
Acetonitrile and concentrated hydrochloric acid mixed solution, dissolved after nitrogen drying with the methanol of 50 μ L chromatographically pures, the ginseng of setting liquid chromatograph
Number is respectively C18Post 4.6mm × 250mm, 25 DEG C of column temperature, mobile phase is volume ratio 42:58 water and the mixed solution of methanol, its
Containing the acetic acid that mass concentration is 1% in reclaimed water, contain the acetic acid that mass concentration is 1%, flow velocity 1mL min in methanol-1, detect ripple
A length of 230nm, the Drawing of Curve concentration-peak area standard curve obtained according to the concentration and liquid chromatograph for preparing sample；
（2）The enrichment analysis of testing sample, adds 1mL vegetable oil to be measured, 9mL n-hexanes and 5 μ L mole in conical flask
Concentration is 2mol L-1Sodium hydroxide solution, then by size for 1cm*2cm dimethyl aminopropyl imidazoles be bonded filter paper solid phase it is micro-
Spe membrane is added in conical flask and sealed, and then takes out dimethylamino in 30 DEG C of vibration absorption 70min with 160r/min rotating speed
Propyl imidazole bonding filter paper solid-phase extraction membrane washing, with 1100 μ L eluent 10min after drying, wherein eluant, eluent is body
Product is than being 50:1 acetonitrile and the mixed solution of concentrated hydrochloric acid, are dissolved with the methanol of 50 μ L chromatographically pures after nitrogen drying, set liquid phase
Chromatographic parameter is respectively C18Post 4.6mm × 250mm, 25 DEG C of column temperature, mobile phase is volume ratio 42:58 water and methanol it is mixed
Containing the acetic acid that mass concentration is 1% in conjunction solution, its reclaimed water, contain the acetic acid that mass concentration is 1%, flow velocity 1mL in methanol
min-1, Detection wavelength is 230nm, and the curve obtained according to liquid chromatograph calculates peak area and according to concentration-peak area standard
Curve calculates the concentration for obtaining paranitrophenol and 2,4- dinitrophenol dinitrophenolates in vegetable oil to be measured.
According to the experimental method and condition determination determined, while analyzing paranitrophenol and 2,4- dinitrophenol dinitrophenolate, mass concentration
In the range of 10-1000 μ g/L, the linearly dependent coefficient of standard curve（r2) it is respectively 0.9935 and 0.9909, for quality
Concentration be in 200 μ g/L paranitrophenol and the vegetable oil of 2,4- dinitrophenol dinitrophenolates relative standard deviation be respectively 2.4% He
5.4%, the 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, principal character and the advantage of the present invention, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (1)
1. a kind of dimethyl aminopropyl imidazoles is bonded the preparation method of filter paper solid-phase extraction membrane, it is characterised in that：It is by 3-
Chloropropyl diethoxy silane coupling agent is by N, and N- dimethyl aminopropyl imidazoles is bonded to formation dimethyl aminopropyl miaow on filter paper
Azoles is bonded filter paper solid-phase extraction membrane, and the dimethyl aminopropyl imidazoles is bonded the specific preparation process of filter paper solid-phase extraction membrane
For：（1）Acetone washing filter paper and room temperature dry it is standby, using 19mL absolute ethyl alcohols as solvent, by 4.7g N, N- dimethyl aminopropyls
It is standby that imidazoles and 6.02g 3- chloropropyl triethoxysilanes obtain product A in 80 DEG C of reaction 24h；（2）12g products A is added
It is 1 to volume ratio:The in the mixed solvent formation mixed system of 4 absolute ethyl alcohol and toluene, take the above-mentioned filter paper dried and with
The distilled water of the quality such as filter paper is squirted, and is then added in above-mentioned mixed system and is reacted 24h in 105 DEG C, and obtained filter paper is first used
Volume ratio is 4:The mixed solution washing of 1 toluene and ethanol, then washed with absolute ethyl alcohol, then it is dried to obtain diformazan in 60 DEG C
Base aminopropyl imidazoles is bonded filter paper solid-phase extraction membrane.
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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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| Title |
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| 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;王香凤等;《分析化学》;20060131;第34卷(第1期);107-110 * |
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