CN108452782A - A kind of preparation and application of magnetic metal organic framework nanometer sheet material - Google Patents
A kind of preparation and application of magnetic metal organic framework nanometer sheet material Download PDFInfo
- Publication number
- CN108452782A CN108452782A CN201810295914.3A CN201810295914A CN108452782A CN 108452782 A CN108452782 A CN 108452782A CN 201810295914 A CN201810295914 A CN 201810295914A CN 108452782 A CN108452782 A CN 108452782A
- Authority
- CN
- China
- Prior art keywords
- sheet material
- methanol
- metal organic
- organic framework
- nanometer sheet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
- B01J20/28—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
- B01J20/28009—Magnetic properties
-
- 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
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
-
- 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
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
Abstract
The invention belongs to solid phase extraction adsorbents technical fields, and in particular to a kind of preparation and application of magnetic metal organic framework nanometer sheet material.Preparation method includes the following steps：1）Nanometer magnetic bead is dispersed in the mixed solution of polyvinylpyrrolidone and chloroform, mechanical agitation 24 hours, collects nanometer magnetic bead, chloroform, methanol cleaning is used in combination, obtains modified Nano magnetic bead, is then dispersed in spare in methanol；2）By step 1）Synthesized modified Nano magnetic bead is dispersed in the methanol mixed solution containing copper nitrate and cobalt nitrate, it is added in the methanol solution containing 2 methylimidazoles under conditions of ultrasonic vibration after being uniformly dispersed, ultrasonic vibration reacts 1 h, then it is cleaned with methanol, magnetic metal organic framework nanometer sheet material is obtained, dispersion is spare in methyl alcohol.The nanometer sheet material of the present invention has more open surfaces, possesses abundant metallic site, and quick separating can be carried out after absorption.
Description
Technical field
The invention belongs to solid phase extraction adsorbents technical fields, and in particular to a kind of magnetic metal organic framework Nano sheet material
The preparation and application of material.
Background technology
Algae is biology most ancient on a kind of earth, their morphological differences is big, simple in structure, typically in ocean
Kind analogy fresh water in type it is more.The nutrition of algae, modes of reproduction are varied, they can quickly increase under suitable conditions
It is long, and water surface is gathered under the action of the buoyancy and hydrographic factor of itself, form the macroscopic algae solution of people, i.e., it is " red
Tide " (Red tide) or " wawter bloom " (Water-bloom)." red tide " or " wawter bloom " is some toxiferous algae classes, its generation mostly
High risks are caused to environment and culture fishery, are considered as worldwide public hazards.Chemical analysis is the normal of domoic acid detection
With method, there is higher sensitivity.It includes high performance liquid chromatography (HPLC), capillary electrophoresis (CE), thin-layer chromatography
Method (TLC) and high performance liquid chromatography-tandem mass method (HPLC-MS/MS) etc..In recent years, due to the Gao Xuan of HPLC-MS/MS
The advantages such as selecting property and high sensitivity make it be increasingly becoming the conventional method of domoic acid analysis detection.But with domoic acid
The continuous expansion of pollution range needs the actual sample type analyzed to become increasingly complex, and the content of domoic acid is also lower and lower,
Therefore it before in instrument, sample introduction is analyzed, needs to carry out a degree of sample pre-treatments, it is sensitive with reduction interference, raising analysis method
Degree, reduces the pollution of instrument, ensures the reliable of analysis result.
Solid Phase Extraction (SPE) is the common pre-treating method of domoic acid separation and concentration, it results from the 1970s
Mid-term is currently used for sample cleanup, the most commonly used method based on solid-phase adsorbent of analyte enrichment method.SPE has
The advantages that easy to operate, solvent consumption is few, but it is easy to block there is also extraction pillar, operating process takes longer etc. lack
Point.In order to overcome these disadvantages, and some Solid Phase Extraction new technologies are derived.The solid-phase adsorbent of magnetization
（MSPE）Just it is being widely used in the separation and concentration of object.This method is substantially the improvement of tradition dSPE methods, than passing
The dSPE methods of system more quickly with simply.In MSPE methods, pass through the help for the externally-applied magnetic field that permanent magnet generates so that magnetic
The separation of the solid-phase adsorbent and sample solution of property becomes simpler.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of magnetic metal organic framework nanometer sheet material
Preparation and application.The nanometer sheet material of the present invention has following advantages：（1）Possess more than conventional metals organic framework material
Open surface, surface utilisation increases；（2）The pattern of bath ball shape can form vortex in adsorption process, be conducive to target
The reservation of analyte；（3）Nanometer sheet material possesses abundant metallic site, possesses with the substance containing polar functional group good
Coordination；（4）Magnetic material can carry out quick separating after absorption.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of magnetic metal organic framework nanometer sheet material, includes the following steps：
1）By 0.3 g nanometer magnetic beads（Diameter is in 300-400 nm）It is dispersed in 300 ml dissolved with 7.5g polyvinylpyrrolidones
In chloroform, mechanical agitation 24 hours is collected magnetic bead and is cleaned with chloroform, methanol, and modified Nano magnetic bead, dispersion is made
In methyl alcohol；
2）By step 1）In synthesized modified Nano magnetic bead be dispersed in dissolved with 0.108 g copper nitrates and 0.26 g cobalt nitrates
7.5 ml methanol in, the methanol solution of 0.41 g/ml 2-methylimidazoles is added after being uniformly dispersed under conditions of ultrasonic vibration
7.5 ml, ultrasonic vibration react 1 h, after cleaned with methanol, magnetic metal organic framework nanometer sheet material is made, is dispersed in methanol
In.
Magnetic metal organic framework nanometer sheet material is in marine organisms sample made from a kind of preparation method as described above
Application in the absorption of middle domoic acid extracts adsorbent using magnetic metal organic framework nanometer sheet material as Magnetic solid phases,
It is measured in conjunction with the triple level four bars mass spectrums of high performance liquid chromatography-；Steps are as follows for concrete application：
1.0 mg magnetic metal organic framework nanometer sheet materials are weighed respectively, are added it to containing a concentration of 25 ng mL-1、
Volume is to adsorb 10 min under room temperature in the domoic acid test solution of 50 mL, isolate material with magnet, supernatant is taken to use
Accela efficient liquid phases system detects cartilage algae with TSQ Quantum Access Max triple quadrupole bar mass spectrometry analyzers
The content of acid observes adsorption effect.
It is an advantage of the invention that：
1）The method of the present invention design is simple, economical, and the magnetic metal organic framework nanometer sheet material of preparation is with a large amount of open
Surface and the pattern favorably adsorbed can quickly detect the content of domoic acid in marine organisms and have good reproducibility
And repeatability, provide possibility for the merchandized handling of the material；
2）Composite material of the present invention is stabilized in water phase and organic phase, can be realized and is used repeatedly, can be greatly
Reduce use cost；
3）Magnetic metal organic framework nanometer sheet material proposed by the present invention.By being modified after modified Nano magnetic bead, in room temperature
Under can be prepared by；Possess a large amount of open surface and active metal sites, and is conducive to adsorb different from traditional material
Pattern, greatly expand the type of functionalized nano material.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of magnetic metal organic framework nanometer sheet material.
Specific implementation mode
Further to disclose rather than the present invention is limited, the present invention is described in further detail below in conjunction with example.
Embodiment 1
The preparation method of magnetic metal organic framework nanometer sheet material, includes the following steps：
1.1 by 0.3 g nanometer magnetic beads（Diameter is in 300-400 nm）It is dispersed in 300 dissolved with 7.5g polyvinylpyrrolidones
In ml chloroforms, mechanical agitation 24 hours is collected magnetic bead and is cleaned with chloroform, methanol, and dispersion is in methyl alcohol；
1.2 are dispersed in modified Nano magnetic bead synthesized in step 1.1 dissolved with 0.108 g copper nitrates and 0.26 g nitric acid
In 7.5 ml methanol of cobalt, the methanol that 0.41 g/ml 2-methylimidazoles are added after being uniformly dispersed under conditions of ultrasonic vibration is molten
7.5 ml of liquid, ultrasonic vibration react 1 h, after cleaned with methanol, dispersion in methyl alcohol.
Application Example 1
The material that embodiment 1 is synthesized extracts adsorbent as Magnetic solid phases, in conjunction with the triple level four bars mass spectrums of high performance liquid chromatography-
(HPLC-TSQ-MS), it is applied to the absorption of domoic acid in marine organisms sample, is as follows：
The magnetic metal organic framework nanometer sheet material for weighing the above-mentioned preparations of 1.0 mg respectively, adds it to containing a concentration of
25 ng mL-1, volume be 50 mL domoic acid test solution in, 10 min are adsorbed under room temperature, material is isolated with magnet,
Supernatant Accela efficient liquid phases system is taken to be analyzed with TSQ Quantum Access Max triple quadrupole bar mass spectrometries
Instrument detects the content of domoic acid, observes adsorption effect；Domoic acid is not detected again in supernatant after absorption.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (7)
1. a kind of preparation method of magnetic metal organic framework nanometer sheet material, it is characterised in that：Include the following steps：
1）Nanometer magnetic bead is dispersed in the mixed solution of polyvinylpyrrolidone and chloroform, mechanical agitation 24 hours, is received
Collect nanometer magnetic bead, chloroform, methanol cleaning is used in combination, obtains modified Nano magnetic bead, is then dispersed in spare in methanol；
2）By step 1）Synthesized modified Nano magnetic bead is dispersed in the methanol mixed solution containing copper nitrate and cobalt nitrate, point
It is added in the methanol solution containing 2-methylimidazole under conditions of ultrasonic vibration after dissipating uniformly, ultrasonic vibration reacts 1 h, then
It is cleaned with methanol, obtains magnetic metal organic framework nanometer sheet material, dispersion is spare in methyl alcohol.
2. the preparation method of magnetic metal organic framework nanometer sheet material according to claim 1, it is characterised in that：Step
1）A diameter of 300-400 nm of the nanometer magnetic bead.
3. the preparation method of magnetic metal organic framework nanometer sheet material according to claim 1, it is characterised in that：Step
1）In the mixed solution of the polyvinylpyrrolidone and chloroform, polyvinylpyrrolidone dosage is 7.5g, three chloromethanes
The dosage of alkane is 300ml.
4. the preparation method of magnetic metal organic framework nanometer sheet material according to claim 1, it is characterised in that：Step
1）The dosage of middle nanometer magnetic bead is 0.3g.
5. the preparation method of magnetic metal organic framework nanometer sheet material according to claim 1, it is characterised in that：Step
2）Described in the methanol mixed solution containing copper nitrate and cobalt nitrate in, the dosage of copper nitrate is 0.108 g, the use of cobalt nitrate
Amount is 0.26 g, and the dosage of methanol is 7.5 ml.
6. the preparation method of magnetic metal organic framework nanometer sheet material according to claim 1, it is characterised in that：Step
2）Described in its a concentration of 0.41 g/ml of the methanol solution containing 2-methylimidazole, dosage be 7.5 ml.
7. magnetic metal organic framework nanometer sheet material made from a kind of preparation method as claimed in any one of claims 1 to 6 exists
Application in marine organisms sample in the absorption of domoic acid, it is characterised in that：With magnetic metal organic framework nanometer sheet material
Adsorbent is extracted as Magnetic solid phases, is measured in conjunction with the triple level four bars mass spectrums of high performance liquid chromatography-.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810295914.3A CN108452782A (en) | 2018-04-04 | 2018-04-04 | A kind of preparation and application of magnetic metal organic framework nanometer sheet material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810295914.3A CN108452782A (en) | 2018-04-04 | 2018-04-04 | A kind of preparation and application of magnetic metal organic framework nanometer sheet material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108452782A true CN108452782A (en) | 2018-08-28 |
Family
ID=63234729
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810295914.3A Pending CN108452782A (en) | 2018-04-04 | 2018-04-04 | A kind of preparation and application of magnetic metal organic framework nanometer sheet material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108452782A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503858A (en) * | 2019-01-17 | 2019-03-22 | 南京大学 | A kind of magnetism sandwich structure metal-organic framework materials and preparation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103638979A (en) * | 2013-11-04 | 2014-03-19 | 北京化工大学 | Magnetic zeolite imidazate metal organic skeletal material, preparation thereof and application to liquid phase condensation catalytic reaction |
| CN104151336A (en) * | 2014-08-08 | 2014-11-19 | 复旦大学 | Preparation method of metal-organic framework compound with hierarchical pore structure |
| CN104174388A (en) * | 2014-08-08 | 2014-12-03 | 复旦大学 | Metal organic frame composite material and preparation method thereof |
| CN105771934A (en) * | 2016-05-06 | 2016-07-20 | 扬州大学 | Preparation method of nanometer magnetic adsorbent with core-shell structure |
-
2018
- 2018-04-04 CN CN201810295914.3A patent/CN108452782A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103638979A (en) * | 2013-11-04 | 2014-03-19 | 北京化工大学 | Magnetic zeolite imidazate metal organic skeletal material, preparation thereof and application to liquid phase condensation catalytic reaction |
| CN104151336A (en) * | 2014-08-08 | 2014-11-19 | 复旦大学 | Preparation method of metal-organic framework compound with hierarchical pore structure |
| CN104174388A (en) * | 2014-08-08 | 2014-12-03 | 复旦大学 | Metal organic frame composite material and preparation method thereof |
| CN105771934A (en) * | 2016-05-06 | 2016-07-20 | 扬州大学 | Preparation method of nanometer magnetic adsorbent with core-shell structure |
Non-Patent Citations (1)
| Title |
|---|
| 林明霞: "磁性固相萃取技术用于贝类中软骨藻酸的分析", 《第21届全国色谱学术报告会及仪器展览会》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109503858A (en) * | 2019-01-17 | 2019-03-22 | 南京大学 | A kind of magnetism sandwich structure metal-organic framework materials and preparation method |
| CN109503858B (en) * | 2019-01-17 | 2021-03-30 | 南京大学 | Magnetic sandwich structure metal organic framework material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Gao et al. | Development and application of vortex-assisted membrane extraction based on metal–organic framework mixed-matrix membrane for the analysis of estrogens in human urine | |
| CN108525635A (en) | A kind of preparation method and applications of the magnetic nitrogen-doped carbon nanometer pipe based on MOF | |
| Ding et al. | n-Octadecylphosphonic acid grafted mesoporous magnetic nanoparticle: Preparation, characterization, and application in magnetic solid-phase extraction | |
| CN108620048A (en) | The amine-modified magnetic microsphere preparation method and application of polyethyleneimine | |
| CN105467026A (en) | Method for detecting perfluorinated compounds in soil and sediments | |
| Liu et al. | On-chip enzymatic microreactor using trypsin-immobilized superparamagnetic nanoparticles for highly efficient proteolysis | |
| CN107860834B (en) | Method for analyzing trace perfluoro compounds by using magnetic organic framework material | |
| Lan et al. | pH-resistant titania hybrid organic–inorganic coating for stir bar sorptive extraction of drugs of abuse in urine samples followed by high performance liquid chromatography–ultraviolet visible detection | |
| Li et al. | Extraction of imide fungicides in water and juice samples using magnetic graphene nanoparticles as adsorbent followed by their determination with gas chromatography and electron capture detection | |
| CN106179237B (en) | A kind of nanofiber and preparation method thereof of extracting and enriching heavy metal ion | |
| CN105498694A (en) | Temperature-sensitive polymer-coated metal organic framework magnetic material and application thereof | |
| CN106706829B (en) | The method that affine in immunity purification-Liquid Chromatography-Tandem Mass Spectrometry measures research of diarrhetic shellfish poisons in shellfish | |
| CN108970585A (en) | The preparation method and application of magnetic metal organic framework composite material a kind of modified after cation | |
| CN105597713B (en) | Magnetic solid-phase extraction material and preparation method and application thereof | |
| CN111487327A (en) | Method for detecting multiple persistent organic chemical pollutants in sample | |
| CN109331795A (en) | A kind of magnetic nanometer composite material and its preparation and application | |
| CN103028351B (en) | Benzene sulfonic acid modified magnetic microsphere and preparation method and application thereof | |
| Avan et al. | CoFe2O4-MWCNTs modified screen printed carbon electrode coupled with magnetic CoFe2O4-MWCNTs based solid phase microextraction for the detection of bisphenol A | |
| Zheng et al. | Novel bimodal porous N-(2-aminoethyl)-3-aminopropyltrimethoxysilane-silica monolithic capillary microextraction and its application to the fractionation of aluminum in rainwater and fruit juice by electrothermal vaporization inductively coupled plasma mass spectrometry | |
| CN106770730B (en) | A kind of methyl mercury and ethyl sclera remodeling method | |
| CN107389835A (en) | The sample-pretreating method of anticoccidial medicament residue in a kind of HPLC MS/MS methods detection animal derived food | |
| CN109459506B (en) | Rapid sample pretreatment method for detecting polychlorinated biphenyl in tea | |
| CN111474248A (en) | Method for determining four preservatives in cosmetics | |
| CN108452782A (en) | A kind of preparation and application of magnetic metal organic framework nanometer sheet material | |
| CN108593792A (en) | Magnetic solid phase extraction-HPLC- the ultraviolet detection methods of environment incretion interferent in water sample |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180828 |