CN109647362A - A kind of preparation method and application of graphene oxide grafting monolithic silica column - Google Patents
A kind of preparation method and application of graphene oxide grafting monolithic silica column Download PDFInfo
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- CN109647362A CN109647362A CN201910151317.8A CN201910151317A CN109647362A CN 109647362 A CN109647362 A CN 109647362A CN 201910151317 A CN201910151317 A CN 201910151317A CN 109647362 A CN109647362 A CN 109647362A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
- B01J20/282—Porous sorbents
- B01J20/285—Porous sorbents based on polymers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2603/00—Systems containing at least three condensed rings
- C07C2603/02—Ortho- or ortho- and peri-condensed systems
- C07C2603/40—Ortho- or ortho- and peri-condensed systems containing four condensed rings
- C07C2603/42—Ortho- or ortho- and peri-condensed systems containing four condensed rings containing only six-membered rings
- C07C2603/50—Pyrenes; Hydrogenated pyrenes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2603/00—Systems containing at least three condensed rings
- C07C2603/02—Ortho- or ortho- and peri-condensed systems
- C07C2603/52—Ortho- or ortho- and peri-condensed systems containing five condensed rings
Abstract
The present invention relates to a kind of preparation method and applications of graphene oxide grafting monolithic silica column, and graphene oxide is grafted on amination monolithic silica column using amidation process, prepare the extraction and separation medium for having good extraction ability to polycyclic aromatic hydrocarbon.With pyrene, benzo [a] pyrene and dibenzo [a, h] anthracene be analysis object, using the sample peak area of liquid chromatographic detection as quantitative basis, graphene oxide grafting monolithic silica column has respectively reached 78.5,98.2,102.4 to the enrichment times of pyrene, benzo [a] pyrene and dibenzo [a, h] anthracene.The present invention keeps easy to operate, mild condition, yield high using amidation process；The graphene oxide grafting monolithic silica column prepared has selectivity good, and matrix is uniform, and permeability is good, the high-efficient advantage of extracting and enriching, separation and enrichment suitable for polycyclic aromatic hydrocarbon.
Description
Technical field
The invention belongs to the preparation fields of solid phase extraction medium in complex system separation analysis, and in particular to a kind of oxidation stone
The preparation method and application of black alkene grafting monolithic silica column.
Background technique
Graphene oxide is a kind of derivative products of graphene, not only possesses biggish specific surface area and stronger pi-electron
Conjugated system, and the functional groups such as its sheet surfaces carboxyl also rich in, hydroxyl, can be repaired by covalent bond or non-covalent bond
Carrier surface is adornd, functional composite material is made, for analyzing the separation and concentration of object.Graphene oxide is to class containing phenyl ring
Closing object has stronger separation and concentration ability, has preferable application prospect in trace PAHs detection.The graphite oxide of the preparations such as Xu
Alkene covalent bonding extracting fiber realizes the extraction detection of polycyclic aromatic hydrocarbons in environmental water sample.
Capillary monolithic column has opposite specific surface area larger, and pressure is small when sample passes through, and mass transfer velocity is fast, analysis time
The advantages such as short.According to the difference of host material, integral post can be divided into Organic Polymer Monolithic Columns and monolithic silica column two major classes.Have
Organic solvent-resistant swelling, pH application range be not narrow for machine polyalcohol integral pole, limits its scope of application.Monolithic silica column is mechanical strong
Degree is high, and high temperature resistant organic solvent-resistant possesses continuous porous structure, biggish specific surface area, and material is easily modified different function
Group is widely used to promote extraction ability in sample pre-treatments and separation analysis field.But current monolithic silica column base
Matter is uneven, and permeability is also bad, and sensitivity is not high, is restricted in the application.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of graphene oxide grafting monolithic silica column and its in polycyclic virtue
Application in the extracting and enriching of hydrocarbon, this method keep easy to operate, mild condition, yield high using amidation process；It prepares
The advantages that integral post has selectivity good, and matrix is uniform, and permeability is good, and extracting and enriching is high-efficient, suitable for polycyclic aromatic hydrocarbon
Separation and enrichment.
The present invention solves its technical problem and adopts the following technical solutions to realize, a kind of oxygen proposed according to the present invention
Graphite alkene is grafted application of the monolithic silica column in polycyclic aromatic hydrocarbon solid phase microextraction, for pyrene, benzo [a] pyrene and dibenzo
The solid phase microextraction of [a, h] anthracene, extraction conditions are as follows: loading solvent is the mixed solution of first alcohol and water, wherein the body of first alcohol and water
Product is than being 1:9, and loading rate is 50 μ L/min, applied sample amount 1mL, and eluent is acetone, and elution rate is 20 μ L/min, elution
Liquid collected volume is 10 μ L.
The present invention solves its technical problem also following technical measures can be used to further realize:
Application of the graphene oxide grafting monolithic silica column above-mentioned in polycyclic aromatic hydrocarbon solid phase microextraction, wherein described
Graphene oxide be grafted monolithic silica column to pyrene, benzo [a] pyrene, dibenzo [a, h] anthracene enrichment times be respectively 78.5,
98.2、102.4。
Application of the graphene oxide grafting monolithic silica column above-mentioned in polycyclic aromatic hydrocarbon solid phase microextraction, in conjunction with HPLC-
UV establishes the quantitative analysis method to polycyclic aromatic hydrocarbon, and the related coefficient of this method is not less than 0.9967, to pyrene, benzo [a] pyrene, two
The detection limit (signal-to-noise ratio S/N=3) of benzo [a, h] anthracene is followed successively by 0.08 μ g/L, 0.02 μ g/L, 0.05 μ g/L, to pyrene, benzo
[a] pyrene, dibenzo [a, h] anthracene quantitative limit (signal-to-noise ratio S/N=10) be followed successively by 0.25 μ g/L, 0.07 μ g/L, 0.16 μ g/L,
Pyrene, benzo [a] pyrene, dibenzo [a, h] anthracene actual sample be averaged recovery of standard addition (n=3) be followed successively by 81.7%-106.9%,
81.5%-107.8%, 82.5%-104.7%, the relative standard deviation (n=3) of pyrene, benzo [a] pyrene, dibenzo [a, h] anthracene
It is followed successively by 1.7%-5.8%, 1.0%-4.5%, 1.5%-6.5%.
Application of the graphene oxide grafting monolithic silica column above-mentioned in polycyclic aromatic hydrocarbon solid phase microextraction, the oxidation stone
Black alkene grafting monolithic silica column the preparation method comprises the following steps:
(1) amination monolithic silica column is prepared:
Tetramethoxy-silicane, polyethylene glycol, urea, acetic acid are stirred into the solution of homogeneous transparent under the conditions of ice-water bath,
After ultrasonic degassing, inject in pretreated capillary, after sealing end in 40 DEG C be aged 20~for 24 hours, then be warming up to 75 DEG C heat preservation 3~
Monolithic silica column is made in 5h, successively rinses removal of impurities with deionized water, anhydrous methanol；Then by amino group donor reagent aminopropyl front three
Oxysilane-methanol solution injects monolithic silica column, in 70 DEG C of 6~8h of reaction after sealing end, obtains amination monolithic silica column, then
It is rinsed with anhydrous methanol spare after cleaning；
(2) graphene oxide grafting monolithic silica column is prepared:
It adds graphene oxide into water, after ultrasound in amination monolithic silica column obtained by dispersion liquid injection step (1), envelope
In 40 DEG C of reaction 6h behind end, graphene oxide is made by amidation process and is grafted monolithic silica column, successively uses deionization later
Water, anhydrous methanol rinse, and remove unreacted residue.
Further, tetramethoxy-silicane described in step (1), polyethylene glycol, urea, acetic acid dosage can be followed successively by
0.90ml, 0.10g, 0.22g, 2ml, the concentration of acetic acid are 0.01mol/L.
Further, tetramethoxy-silicane, polyethylene glycol, urea, acetic acid dosage can successively according to 0.90mL, 0.10g,
0.22g, 2mL are increasedd or decreased in identical multiple.
Further, aminopropyl in amino group donor reagent aminopropyl trimethoxysilane described in step (1)-methanol solution
The volume ratio of trimethoxy silane and anhydrous methanol is 3:7；The rate that the amino group donor reagent injects monolithic silica column is 50 μ L/
Min, dosage 1mL.
It further, is that graphene oxide aqueous dispersions are injected into amination silica gel with the rate of 30 μ L/min in step (2)
In integral post.
Compared with prior art, the invention has the following advantages that
The graphene oxide that the present invention is prepared is grafted monolithic silica column, and matrix is uniform, and permeability is good, and amidation is anti-
The application answered keeps modification easily operated, and reaction conversion ratio is higher.It is found in polycyclic aromatic hydrocarbon enrichment research, graphite oxide
Alkene grafting monolithic silica column has high bioaccumulation efficiency and highly selective, and due to active group-NH2Presence, be integral post
Post column derivatization provide more possibility.The new side provided by the invention for preparing graphene oxide grafting monolithic silica column
Method overcomes Organic Polymer Monolithic Columns not organic solvent-resistant swelling, the problems such as pH application range is narrow, final gained graphite oxide
Alkene, which is grafted monolithic silica column, has selectivity good, and matrix is uniform, and permeability is good, the high advantage of bioaccumulation efficiency, is suitable for polycyclic
The separation and enrichment of aromatic hydrocarbons.
Detailed description of the invention
Fig. 1 is the raman spectrum of (a) and (b) monolithic silica column after modification before graphene oxide modification；
Fig. 2 is the scanning electron microscope (SEM) photograph of monolithic silica column before graphene oxide is modified；
Fig. 3 is the scanning electron microscope (SEM) photograph of monolithic silica column after graphene oxide modification；
Fig. 4 is that graphene oxide is grafted monolithic silica column to pyrene (b1), benzo [a] pyrene (b2) and dibenzo [a, h] anthracene
(b3) liquid chromatogram of (a) and (b) after enrichment before mixed standard solution is enriched with.
Specific embodiment
The technological means and technical effect taken for the present invention is further explained, with reference to embodiments, to the present invention into
Row is described in detail.
The preparation method of a kind of graphene oxide grafting monolithic silica column, using amidation process by graphite oxide alkenyl group
It is grafted on amination monolithic silica column, prepares and silica gel is grafted to the graphene oxide that aromatic hydrocarbon group has good extraction ability
Integral post.
As preferrred embodiment of the present invention, the amination monolithic silica column the preparation method comprises the following steps: by tetramethoxy
Silane, polyethylene glycol, urea, acetic acid stir into homogeneous transparent solution under the conditions of ice-water bath, and inject processed capillary
In, control column temperature is reacted, and monolithic silica column is made, is then further modified using aminopropyl trimethoxysilane and obtains ammonia
Base monolithic silica column.The amidation process process are as follows: it is whole that the aqueous dispersions of graphene oxide are injected into amination silica gel
In scapus, graphene oxide grafting monolithic silica column can be obtained through isothermal reaction.
The graphene oxide grafting monolithic silica column of preparation method preparation of the present invention is micro- in the solid phase of polycyclic aromatic hydrocarbon
Application in extraction, extraction process are as follows: with pyrene, the methanol/water (methanol: water volume ratio of benzo [a] pyrene and dibenzo [a, h] anthracene
It is analysis object for 1:9) solution, using the sample peak area of liquid chromatographic detection as quantitative basis, extraction conditions is as follows: loading is molten
Agent is methanol/water mixed solution, wherein the volume ratio of methanol and water is 1:9, and loading rate is 50 μ L/min, and applied sample amount is
1mL, eluent are acetone, and elution rate is 20 μ L/min, and eluent collected volume is 10 μ L.
To be clearer and more comprehensible the contents of the present invention, below in conjunction with specific embodiment, the present invention will be described in detail.
Embodiment 1
Preparation method about graphene oxide grafting monolithic silica column
Step 1: the pretreatment of capillary
Quartz capillary use first 1moL/L NaOH activate, then successively with 1moL/L HCl and deionized water rinse to
Neutrality is dried with nitrogen spare.
Step 2: the preparation of graphene oxide
Mixed acid (H is added in 1.0g graphite powder2SO4And H3PO4Volume ratio is the mixed acid of 9:1) 134mL, machinery stirs
It mixes down and is slowly added to 6.0g KMnO4, 50 DEG C of oil baths reaction 30h.Reaction terminates to pour into 150mL ice water after being cooled to room temperature, is added dropwise
8mL 30%H2O2.It successively is washed till neutrality with 10%HCl, dehydrated alcohol, deionized water, graphite oxide is obtained after drying.Take appropriate oxygen
Graphite, through ultrasonic disperse, both obtains graphene oxide aqueous dispersions in deionized water.
Step 3: the preparation of amination monolithic silica column
0.90mL TMOS, 0.10g PEG and 0.22g Urea is taken to mix with 2mL 0.01mol/L HAc, ice bath stirring is extremely
Clear, after ultrasonic degassing, injection 8cm long is pre-processed in capillary, 40 DEG C of ageing 20h after sealing end, then is warming up to 75 DEG C of guarantors
3h is held, monolithic silica column is made, successively rinses removal of impurities with deionized water and anhydrous methanol.Then by 1mL amino group donor reagent ammonia
Propyl trimethoxy silicane (APTMS)-methanol solution injects monolithic silica column, 70 DEG C of reactions after sealing end with the rate of 50 μ L/min
6h obtains amination monolithic silica column, is rinsed with anhydrous methanol spare after cleaning.The amino group donor reagent aminopropyl trimethoxy
Silane (APTMS)-methanol solution is that aminopropyl trimethoxysilane (APTMS) is dissolved in anhydrous methanol, aminopropyl trimethoxy
The volume ratio of base silane (APTMS) and anhydrous methanol is 3:7.
Step 4: the preparation of graphene oxide grafting monolithic silica column
The graphene oxide aqueous dispersions 1mL of 0.02mg/mL is whole with the rate injection amination silica gel of 30 μ L/min
Column, 40 DEG C of reaction 6h after sealing end are made graphene oxide by amidation process and are grafted monolithic silica column, successively spend later from
Sub- water, anhydrous methanol rinse, and remove unreacted graphene oxide.
Fig. 1 middle line a and line b is respectively the raman spectrum that graphene oxide (GO) is grafted forward and backward monolithic silica column, line b table
It is bright: after GO grafting, in 1350cm-1And 1600cm-1There is two apparent absorption peaks, the peak characteristic peak D and G of respectively GO
Peak.Show that GO is successfully grafted to monolithic silica column surface.
Fig. 2 and Fig. 3 is respectively the scanning electron microscope (SEM) photograph of graphene oxide grafting front and back monolithic silica column, and Fig. 3 shows: GO grafting
Afterwards, there is a large amount of fold in monolithic silica column material surface, illustrates that GO successfully grafts on monolithic silica column surface.
Embodiment 2
About application of the graphene oxide grafting monolithic silica column in the solid phase microextraction of polycyclic aromatic hydrocarbon
The foundation of extracting process: extracting process is molten with the hybrid standard of pyrene, benzo [a] pyrene and dibenzo [a, h] anthracene three
Liquid is analysis object, and pyrene, benzo [a] pyrene and dibenzo [a, h] anthracene three are dissolved in methanol/water solution (methanol: water volume
Than carrying out under following extraction conditions for 1:9) using the sample peak area of liquid chromatographic detection as quantitative basis: loading solvent is
Volume ratio is the methanol/water mixed solution of 1:9, and loading rate is 50 μ L/min, and applied sample amount 1mL, eluent is acetone, elution
Rate is 20 μ L/min, and eluent collected volume is 10 μ L.Under optimal conditions, it is whole to investigate graphene oxide grafting silica gel
Concentration effect of the column to pyrene, benzo [a] pyrene and dibenzo [a, h] anthracene, the results showed that, integral post is to pyrene, benzo [a] pyrene and hexichol
And the enrichment times of [a, h] anthracene have respectively reached 78.5,98.2,102.4.
Fig. 4 middle line a and line b is respectively graphene oxide grafting monolithic silica column to pyrene (label 1 in line b), benzo [a] pyrene
Liquid chromatogram before the enrichment of (label 2 in line b) and dibenzo [a, h] anthracene (label 3 in line b) mixed standard solution and after enrichment
Figure, after line b shows enrichment, chromatographic peak area is significantly increased.
The present invention is established in conjunction with HPLC-UV to polycyclic virtue using graphene oxide grafting monolithic silica column as spe medium
The quantitative analysis method of hydrocarbon (PAHs).It is analyzed with 0.1-150 μ g/L series standard solution, using concentration as abscissa, extraction
Sample chromatogram peak area is that ordinate carries out linear regression analysis afterwards, determines the standard curve, linear of polycyclic aromatic hydrocarbon (PAHs)
Range, detection limit (LOD, S/N=3) and quantitative limit (LOQ, S/N=10), as a result such as table 1.Experiment measures the phase relation of this method
Number is not less than 0.9967, and detection limit is between 0.02-0.08 μ g/L, and quantitative limit is between 0.07-0.25 μ g/L.Pyrene, benzo [a]
Pyrene, dibenzo [a, h] anthracene actual sample recovery of standard addition (n=3) that is averaged are respectively 81.7%-106.9%, 81.5%-
107.8%, 82.5%-104.7%, relative standard deviation (RSD) is respectively 1.7%-5.8%, 1.0%-4.5%, 1.5%-
6.5% (n=3).
The standard curve of 1. 3 kinds of PAHs of table, related coefficient, the range of linearity, detection limit, quantitative limit result
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form, appoint
What those skilled in the art, without departing from the scope of the present invention, according to the technical essence of the invention to
Any simple modification, equivalent change and modification made by upper embodiment, all of which are still within the scope of the technical scheme of the invention.
Claims (8)
1. application of a kind of graphene oxide grafting monolithic silica column in polycyclic aromatic hydrocarbon solid phase microextraction, for pyrene, benzo
The solid phase microextraction of [a] pyrene and dibenzo [a, h] anthracene, extraction conditions are as follows: loading solvent is the mixed solution of first alcohol and water,
In, the volume ratio of first alcohol and water is 1:9, and loading rate is 50 μ L/min, and applied sample amount 1mL, eluent is acetone, elution rate
For 20 μ L/min, eluent collected volume is 10 μ L.
2. application of the graphene oxide grafting monolithic silica column as described in claim 1 in polycyclic aromatic hydrocarbon solid phase microextraction,
It is characterized by: graphene oxide grafting monolithic silica column to pyrene, benzo [a] pyrene, dibenzo [a, h] anthracene enrichment times
Respectively 78.5,98.2,102.4.
3. application of the graphene oxide grafting monolithic silica column as described in claim 1 in polycyclic aromatic hydrocarbon solid phase microextraction,
It is characterized by: establishing the quantitative analysis method to polycyclic aromatic hydrocarbon in conjunction with HPLC-UV, the related coefficient of this method is not less than
0.9967,0.08 μ g/L, 0.02 μ g/L, 0.05 μ g/L are followed successively by the detection limit of pyrene, benzo [a] pyrene, dibenzo [a, h] anthracene；
0.25 μ g/L, 0.07 μ g/L, 0.16 μ g/L are followed successively by the quantitative limit of pyrene, benzo [a] pyrene, dibenzo [a, h] anthracene；Pyrene, benzo
[a] pyrene, dibenzo [a, h] anthracene actual sample be averaged recovery of standard addition be followed successively by 81.7%-106.9%, 81.5%-107.8%,
82.5%-104.7%, pyrene, benzo [a] pyrene, dibenzo [a, h] anthracene relative standard deviation be followed successively by 1.7%-5.8%,
1.0%-4.5%, 1.5%-6.5%.
4. application of the graphene oxide grafting monolithic silica column as described in claim 1 in polycyclic aromatic hydrocarbon solid phase microextraction,
It is characterized by: graphene oxide grafting monolithic silica column the preparation method comprises the following steps:
(1) amination monolithic silica column is prepared:
Tetramethoxy-silicane, polyethylene glycol, urea, acetic acid are stirred into the solution of homogeneous transparent under the conditions of ice-water bath, ultrasound
After degassing, inject in pretreated capillary, it is aged in 40 DEG C 20 after sealing end~for 24 hours, then it is warming up to 75 DEG C of constant temperature 3~5h systems
Monolithic silica column is obtained, successively rinses removal of impurities with deionized water, anhydrous methanol；Then by amino group donor reagent aminopropyl trimethoxy
Silane-methanol solution injects monolithic silica column, in 70 DEG C of 6~8h of reaction after sealing end, obtains amination monolithic silica column, then use nothing
It is spare after water methanol flushing removal of impurities；
(2) graphene oxide grafting monolithic silica column is prepared:
Add graphene oxide into water, after ultrasonic disperse in amination monolithic silica column obtained by injection step (1), after sealing end in
40 DEG C of reaction 6h are made graphene oxide by amidation process and are grafted monolithic silica column, successively use deionized water, methanol later
It rinses, removes residual reactant.
5. application of the graphene oxide grafting monolithic silica column as claimed in claim 4 in polycyclic aromatic hydrocarbon solid phase microextraction,
It is characterized in that the dosage of tetramethoxy-silicane described in step (1), polyethylene glycol, urea, acetic acid be followed successively by 0.90mL,
0.10g, 0.22g, 2mL, the concentration of acetic acid are 0.01mol/L.
6. application of the graphene oxide grafting monolithic silica column as claimed in claim 5 in polycyclic aromatic hydrocarbon solid phase microextraction,
It is characterized in that the dosage of tetramethoxy-silicane, polyethylene glycol, urea, acetic acid is successively according to 0.90ml, 0.10g, 0.22g, 2ml
It is increasedd or decreased in identical multiple.
7. application of the graphene oxide grafting monolithic silica column as claimed in claim 4 in polycyclic aromatic hydrocarbon solid phase microextraction,
It is characterized in that aminopropyl front three in amino group donor reagent aminopropyl trimethoxysilane described in step (1)-methanol solution
Oxysilane and the volume ratio of anhydrous methanol are 3:7；The rate that the amino group donor reagent injects monolithic silica column is 50 μ L/min,
Dosage is 1mL.
8. application of the graphene oxide grafting monolithic silica column as claimed in claim 4 in polycyclic aromatic hydrocarbon solid phase microextraction,
It is characterized in that being that graphene oxide aqueous dispersions are injected amination monolithic silica column with the rate of 30 μ L/min in step (2)
In.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341579A (en) * | 2020-11-26 | 2021-02-09 | 蚌埠市华东生物科技有限公司 | Adsorption resin for separating and purifying stevioside and application thereof |
| CN113373189A (en) * | 2021-06-01 | 2021-09-10 | 南京师范大学 | Method and device for continuously producing ellagic acid |
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