CN108212091A - Ordered mesoporous carbon material of 18 carbon modification and its preparation method and application - Google Patents
Ordered mesoporous carbon material of 18 carbon modification and its preparation method and application Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 43
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 37
- 230000004048 modification Effects 0.000 title claims abstract description 16
- 238000012986 modification Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000243 solution Substances 0.000 claims abstract description 16
- SLYCYWCVSGPDFR-UHFFFAOYSA-N octadecyltrimethoxysilane Chemical compound CCCCCCCCCCCCCCCCCC[Si](OC)(OC)OC SLYCYWCVSGPDFR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000967 suction filtration Methods 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 13
- MUMGGOZAMZWBJJ-DYKIIFRCSA-N Testostosterone Chemical compound O=C1CC[C@]2(C)[C@H]3CC[C@](C)([C@H](CC4)O)[C@@H]4[C@@H]3CCC2=C1 MUMGGOZAMZWBJJ-DYKIIFRCSA-N 0.000 claims description 12
- 150000003384 small molecules Chemical class 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 239000008280 blood Substances 0.000 claims description 6
- 210000004369 blood Anatomy 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- QMGVPVSNSZLJIA-FVWCLLPLSA-N strychnine Chemical compound O([C@H]1CC(N([C@H]2[C@H]1[C@H]1C3)C=4C5=CC=CC=4)=O)CC=C1CN1[C@@H]3[C@]25CC1 QMGVPVSNSZLJIA-FVWCLLPLSA-N 0.000 claims description 6
- 229960003604 testosterone Drugs 0.000 claims description 6
- FNYLWPVRPXGIIP-UHFFFAOYSA-N Triamterene Chemical group NC1=NC2=NC(N)=NC(N)=C2N=C1C1=CC=CC=C1 FNYLWPVRPXGIIP-UHFFFAOYSA-N 0.000 claims description 5
- MEHHPFQKXOUFFV-OWSLCNJRSA-N trenbolone Chemical compound C1CC(=O)C=C2CC[C@@H]([C@H]3[C@@](C)([C@H](CC3)O)C=C3)C3=C21 MEHHPFQKXOUFFV-OWSLCNJRSA-N 0.000 claims description 5
- 229960000312 trenbolone Drugs 0.000 claims description 5
- 229960001288 triamterene Drugs 0.000 claims description 5
- STJMRWALKKWQGH-UHFFFAOYSA-N clenbuterol Chemical compound CC(C)(C)NCC(O)C1=CC(Cl)=C(N)C(Cl)=C1 STJMRWALKKWQGH-UHFFFAOYSA-N 0.000 claims description 4
- 229960001117 clenbuterol Drugs 0.000 claims description 4
- 239000003599 detergent Substances 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- QMGVPVSNSZLJIA-UHFFFAOYSA-N Nux Vomica Natural products C1C2C3C4N(C=5C6=CC=CC=5)C(=O)CC3OCC=C2CN2C1C46CC2 QMGVPVSNSZLJIA-UHFFFAOYSA-N 0.000 claims description 3
- 241001279009 Strychnos toxifera Species 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229960005453 strychnine Drugs 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 16
- 238000001179 sorption measurement Methods 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 10
- 239000011148 porous material Substances 0.000 abstract description 4
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- 238000007306 functionalization reaction Methods 0.000 abstract 1
- 230000003993 interaction Effects 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 239000005416 organic matter Substances 0.000 abstract 1
- GCKMFJBGXUYNAG-UHFFFAOYSA-N 17alpha-methyltestosterone Natural products C1CC2=CC(=O)CCC2(C)C2C1C1CCC(C)(O)C1(C)CC2 GCKMFJBGXUYNAG-UHFFFAOYSA-N 0.000 description 4
- GCKMFJBGXUYNAG-HLXURNFRSA-N Methyltestosterone Chemical compound C1CC2=CC(=O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@](C)(O)[C@@]1(C)CC2 GCKMFJBGXUYNAG-HLXURNFRSA-N 0.000 description 4
- 229960001566 methyltestosterone Drugs 0.000 description 4
- 238000001819 mass spectrum Methods 0.000 description 3
- 239000013335 mesoporous material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910008051 Si-OH Inorganic materials 0.000 description 2
- 229910006358 Si—OH Inorganic materials 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 150000001793 charged compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007717 exclusion Effects 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000001840 matrix-assisted laser desorption--ionisation time-of-flight mass spectrometry Methods 0.000 description 2
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 2
- 229910014571 C—O—Si Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- SXFKQMHYKBDBKL-UHFFFAOYSA-N methoxy(octadecyl)silane Chemical compound CCCCCCCCCCCCCCCCCC[SiH2]OC SXFKQMHYKBDBKL-UHFFFAOYSA-N 0.000 description 1
- -1 methoxyl group Chemical group 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229940038384 octadecane Drugs 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to functionalization sorbing material fields, provide the preparation method of ordered mesoporous carbon material that a kind of 18 carbon (C18) are modified, include the following steps：1) octadecyl trimethoxysilane is added in toluene solution, mixing is stirred at room temperature；2) it adds in ordered mesoporous carbon material into the solution after above-mentioned stirring and ultrasonic disperse is uniform；3) mixed solution is flowed back for 24 hours at 180 DEG C ± 5 DEG C；4) mixed liquor is filtered with Suction filtration device after taking out reaction, is washed and is dried, you can obtains the ordered mesoporous carbon material of 18 carbon (C18) modification.Ordered mesoporous carbon material made from the embodiment of the present application can enhance its adsorption capacity to organic matter by carbon interchain interaction and hydrophobic effect, and the nano pore that ordered mesopore carbon has can exclude the interference of macromolecular substances by molecular dimension effect, so as to achieve the purpose that selectively to adsorb small organic molecule.
Description
Technical field
The present invention relates to a kind of preparation methods of the sorbing material of functional ordered mesopore carbon, and in particular to a kind of octadecane
Base trimethoxy silane (C18) modifies the preparation method of ordered mesopore carbon.
Background technology
Ordered mesoporous material is the rapidly growing novel nano structure material nineties in last century.Ordered mesoporous material due to
The duct of its high-sequential, big specific surface area, high porosity, narrow pore-size distribution, the pore structure of rule, controllable aperture
Size, higher thermal stability and chemical stability and dimensional effect, skin effect, the amount shown due to its unique texture
The characteristics such as sub- confinement effect make it obtain important application, therefore one in catalyst carrier, hydrogen storage material, electrode material etc.
It is born and just obtains the great attention of the educational circles such as internationalization, physics, material and biology, and rapidly develops as research interdisciplinary
Hot spot it-.
Ordered mesopore carbon is a kind of novel non-silicon-based mesoporous material.The nano-pore structure of the uniform and ordered of ordered mesopore carbon
So that it has " size exclusion " effect, the compound in the aperture less than or equal to it can be adsorbed, and excludes the dry of macromolecular
It disturbs.Compared with pure mesoporous silicon material, ordered mesoporous carbon material shows special property, and such as huge specific surface area is (up to
2500m2/ g) and pore volume (up to 2.25cm3/ g), high-sequential and adjustable aperture, uniform mass transfer ability, low diffusion
Resistance, high-adsorption-capacity, good biocompatibility and corrosion resistance etc..Therefore it is wide often as a kind of excellent sorbing material
The general adsorption and enrichment applied to heavy metal ion, organic pollution and large biological molecule etc. is with detaching.
Present inventor has found under study for action, although ordered mesopore carbon has size selection adsorption capacity, due to it
Surface is electrically charged more, and the adsorption capacity of stronger to hydrophobicity or Long carbon chain type compound is weaker, therefore limits it
Using.
Invention content
The embodiment of the present application provides a kind of novel absorption material based on 18 carbon modification ordered mesopore carbon, and tradition is overcome to have
The shortcomings that sequence meso-porous carbon material is stronger to hydrophobicity or the adsorption capacity of the compound of Long carbon chain type is weaker, enhances and is orderly situated between
The adsorption capacity of hole carbon material, expands application range.
The present invention provides the preparation method of ordered mesoporous carbon material that a kind of 18 carbon (C18) are modified, and includes the following steps：
1) octadecyl trimethoxysilane is added in toluene solution, mixing is stirred at room temperature；
2) it adds in ordered mesoporous carbon material into the solution after above-mentioned stirring and ultrasonic disperse is uniform；
3) mixed solution is flowed back for 24 hours at 180 DEG C ± 5 DEG C；
4) mixed liquor is filtered with Suction filtration device after taking out reaction, is washed and is dried, you can obtains 18 carbon (C18) modification
Ordered mesoporous carbon material.
Further, the detergent used in the step 4) is toluene.
Further, the drying temperature in the step 4) is 120 DEG C.
Further, a concentration of 0.35mmoL/L of the octadecyl trimethoxysilane in toluene solution.
Further, a concentration of 10g/L of the ordered mesoporous carbon material in toluene solution.
Further, the mass ratio 1 of the octadecyl trimethoxysilane and the ordered mesoporous carbon material：15.
Further, the ultrasonic temperature in the step 2) is 25 DEG C, ultrasonic time 20min, supersonic frequency 40Hz, ultrasound
Power 600W.
On the other hand, the ordered mesoporous carbon material that 18 carbon (C18) according to made from the above method are modified, applied to hydrophobic
The absorption of stronger or Long carbon chain type the compound of property.
On the other hand, the ordered mesoporous carbon material that 18 carbon (C18) according to made from the above method are modified, applied to people
Excitant small molecule in whole blood is adsorbed, the excitant small molecule for triamterene, Trenbolone, testosterone, methyltestosterone,
Six kinds of excitant small molecules of Clenbuterol and strychnine.
On the other hand, the present invention provides the ordered mesoporous carbon material that a kind of 18 carbon (C18) are modified, the ordered mesopore carbon
H on the hydroxyl of material surface is by octadecyl trimethoxysilaneSubstitution.
Ordered mesopore carbon is modified based on 18 carbon prepared by the present invention, can be extracted by hydrophobicity effect unmodified
Ordered mesopore carbon is difficult to that the hydrophobicity adsorbed is stronger or the compound of Long carbon chain type, and selectivity is wider.
Description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is this hair
Some bright embodiments, for those of ordinary skill in the art, without creative efforts, can be with root
Other attached drawings are obtained according to these attached drawings.
Figure 1A -1B are a kind of preparation of the ordered mesoporous carbon material of 18 carbon (C18) modification provided in an embodiment of the present invention
The transmission electron microscope comparison chart of C18-CMK8 and CMK8 and material prepared by method；
Fig. 2A -2D are that the present invention applies the preparation side of the ordered mesoporous carbon material of 18 carbon of one kind (C18) modification that example provides
C18-CMK8 prepared by method flies the substance assistant laser desorpted ionized of target analytes in people's whole blood with CMK8 sorbing materials
Row time mass spectrum (MALDI-TOF MS) collection of illustrative plates.
Specific embodiment
Purpose, technical scheme and advantage to make the embodiment of the present invention are clearer, below in conjunction with the embodiment of the present invention
In attached drawing, clear, complete description is carried out to the technical solution in the embodiment of the present invention, it is clear that described embodiment is
Part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
All other embodiments obtained without making creative work shall fall within the protection scope of the present invention.
The embodiment of the present application provides the preparation method of ordered mesoporous carbon material that a kind of 18 carbon (C18) are modified, including such as
Lower step：
1) octadecyl trimethoxysilane is added in toluene solution, mixing is stirred at room temperature, toluene solution is as reaction
Solvent provides the environment of a high pressure for reaction；
2) it adds in ordered mesoporous carbon material into the solution after above-mentioned stirring and ultrasonic disperse is uniform；
3) mixed solution is flowed back for 24 hours at 180 DEG C ± 5 DEG C；
4) mixed liquor is filtered with Suction filtration device after taking out reaction, is washed and is dried, you can obtains 18 carbon (C18) modification
Ordered mesoporous carbon material.
Wherein, for the detergent used in the step 4) for toluene, the toluene is not anti-for removing removal as detergent
The octadecyl trimethoxysilane answered, drying temperature is 120 DEG C in the step 4), to remove remaining toluene in product.
Wherein, a concentration of 0.35mmoL/L of the octadecyl trimethoxysilane in toluene solution, it is described orderly
A concentration of 10g/L of the meso-porous carbon material in toluene solution.
Wherein, the mass ratio 1 of the octadecyl trimethoxysilane and the ordered mesoporous carbon material：15.
Wherein, the ultrasonic temperature in the step 2) is 25 DEG C, ultrasonic time 20min, supersonic frequency 40Hz, ultrasonic power
600W。
In the embodiment of the present application, it using different meso-porous carbon materials, can also prepare with different meso-hole structures and hole
The sorbing material of diameter size meets different actual demands.
As can be seen that C18-CMK8 still maintains original meso-hole structure after modification from Figure 1A and Figure 1B, it ensure that
" size exclusion " effect is played during adsorbed target analyte, removes the interference of macromolecular.
Ordered mesopore carbon is modified based on 18 carbon prepared by the present invention, can be extracted by hydrophobicity effect unmodified
Ordered mesopore carbon is difficult to that the hydrophobicity adsorbed is stronger or the compound of Long carbon chain type, and selectivity is wider.In addition, based on ten
Eight carbon modification ordered mesopore carbon has higher phosphorus content and high hydrophobicity, can greatly increase volume containing the sample and the rate of recovery, Gao Han
Carbon amounts can also be resistant to extreme pH value simultaneously.But also with preparation process is few, device is simple, can be mass-produced, Yi Shi
The advantages that existing commercialization.Therefore, above-mentioned preparation method based on 18 carbon modification ordered mesopore carbon have broad application prospects,
Such as purification, extraction, the pollutant in concentration environmental water sample such as the pesticide residue in polycyclic aromatic hydrocarbon, food and drink and biology flow
Drug and metabolin in body etc..
With reference to specific example, the present invention will be described in detail.Protection scope of the present invention is not with specific embodiment party
Formula is limited, but is defined in the claims.
Embodiment 1：
It prepares a kind of 18 carbon that are based on and modifies ordered mesopore carbon, method is as follows：
0.15mL octadecyl trimethoxysilane reagents are added in 20mL toluene solutions simultaneously room temperature magnetic agitation
Then 10min mixings add in ordered mesoporous carbon material CMK-8, the ultrasonic disperse 20min of 0.2g, then flow back at 185 DEG C anti-
Should for 24 hours, the mixed liquor after reaction is filtered with Suction filtration device, and toluene washing dries 12h at 120 DEG C, and obtained product is C18
The mesoporous carbon adsorbing materials of CMK-8 (C18-CMK8) of modification.
The reaction principle of the embodiment of the present invention 1：
3 methoxyl group (- OCH being connected in octadecyl methoxy silane with silicon3) it is hydrolyzed into silicone hydroxyl (Si- first
OH)；Then Si-OH forms hydrogen bond with the hydroxyl (- OH) on ordered mesoporous carbon material surface；With dehydration during being heated to reflux
Reaction, the Si-OH of silane form a covalent bond C-O-Si connection in order mesoporous carbon surface.
Chemical equation is as follows：
The CMK-8 mesoporous carbons modified using the C18 prepared by example 1 is sorbing materials, to small point of the excitant in people's whole blood
Son is adsorbed, and adsorbed excitant is finally detected using MALDI-TOF MS, and the adsorption effect of sorbing material is evaluated with this.
Selected excitant small molecule is that triamterene, Trenbolone, testosterone, methyltestosterone, Clenbuterol and six kinds of excitants of strychnine are small
Molecule.
In the application, sorbing material C18-CMK8 is formulated as aqueous solution, a concentration of 10g/L.
In the application, the volume ratio for adding in C18-CMK8 and people's whole blood sample is 10:1.
In the application, adsorption temp is 25 DEG C, adsorption time 1h.
In the application, compare adsorption effect using unmodified CMK-8.
Referring to Fig. 2A -2D, (experiment analyzes in people's whole blood six kinds to experimental result by adsorbent of CMK-8 and C18-CMK8 respectively
Mass spectrum (MS) figure in excitant, wherein：(A) it does not extract, (B) mark-on is not extracted through C18-CMK8, and (C) mark-on extracts through CMK-8
Take and (D) mark-on extracted through C18-CMK8), wherein, triamterene, Trenbolone, Clenbuterol, testosterone, methyltestosterone and scholar
Peaceful characteristic peak corresponds to m/z 254.1 respectively；M/z 270.2 and 455.4；m/z 277；M/z 288.2 and 473.5；m/z
302.2 and 487.5；m/z 335.2.From fig. 1, it can be seen that result shows not enriched, any signal can't detect completely.And pass through
After the enrichment of C18-CMK8 sorption extractions, the molecular ion characteristic peak of all target analytes successfully is detected from complex sample
Value, and detection triamterene, Trenbolone, testosterone, four kinds of methyltestosterone are only capable of after CMK8 adsorption and enrichments.Compared with CMK8, C18-
CMK8 can detect more excitant small molecules and peak intensity higher.Illustrate that C18-CMK8 adsorbents have higher absorption
Efficiency and wider array of adsorption range, show good absorption property.
Material of the present invention has the beneficial effect that：
1st, C18-CMK8 can effectively remove the disturbing effect of sample substrate, than unmodified CMK-8 peak intensities more
Height, background are cleaner.
2nd, C18-CMK8 can successfully be detected the molecular ion characteristic peaks of all target analytes from complex sample,
And unmodified CMK-8 is only capable of detecting a part.
Prepared can be used as a kind of sorbing material based on 18 carbon modification ordered mesopore carbon, more orderly than unmodified
The absorption property of meso-porous carbon material is stronger.
The foregoing is merely presently preferred embodiments of the present invention, it is noted that for those skilled in the art
For, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (10)
1. the preparation method of ordered mesoporous carbon material that a kind of 18 carbon (C18) are modified, which is characterized in that include the following steps：
1) octadecyl trimethoxysilane is added in toluene solution, mixing is stirred at room temperature；
2) it adds in ordered mesoporous carbon material into the solution after above-mentioned stirring and ultrasonic disperse is uniform；
3) mixed solution is flowed back for 24 hours at 180 DEG C ± 5 DEG C；
4) mixed liquor is filtered with Suction filtration device after taking out reaction, is washed and is dried, you can obtains the orderly of 18 carbon (C18) modification
Meso-porous carbon material.
2. method according to claim 1, which is characterized in that the detergent used in the step 4) is toluene.
3. method according to claim 1 or claim 2, which is characterized in that the drying temperature in the step 4) is 120 DEG C.
4. according to one of claim 1-3 the methods, which is characterized in that the octadecyl trimethoxysilane is molten in toluene
A concentration of 0.35mmoL/L in liquid.
5. according to one of claim 1-4 the methods, which is characterized in that the ordered mesoporous carbon material is in toluene solution
A concentration of 10g/L.
6. according to one of claim 1-5 the methods, which is characterized in that the octadecyl trimethoxysilane has with described
The mass ratio 1 of sequence meso-porous carbon material：15.
7. according to one of claim 1-6 the methods, which is characterized in that the ultrasonic temperature in the step 2) is 25 DEG C, is surpassed
Sound time 20min, supersonic frequency 40Hz, ultrasonic power 600W.
8. according to the ordered mesoporous carbon material that 18 carbon (C18) made from one of claim 1-7 the methods are modified, it is applied to
Hydrophobicity is stronger or the absorption of the compound of Long carbon chain type.
9. according to the ordered mesoporous carbon material that 18 carbon (C18) made from one of claim 1-7 the methods are modified, it is applied to
Excitant small molecule in people's whole blood is adsorbed, the excitant small molecule is triamterene, Trenbolone, testosterone, methyl
Six kinds of testosterone, Clenbuterol and strychnine excitant small molecules.
A kind of 10. ordered mesoporous carbon material that 18 carbon (C18) are modified, which is characterized in that the ordered mesoporous carbon material surface
Hydroxyl on H by octadecyl trimethoxysilaneReplaced.
Priority Applications (1)
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| CN110292911A (en) * | 2019-07-16 | 2019-10-01 | 四川长晏科技有限公司 | A kind of modified hectorite and preparation method thereof |
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