CN101721840A - Device and method for preparing chromatographic column made of magnetic filling material - Google Patents
Device and method for preparing chromatographic column made of magnetic filling material Download PDFInfo
- Publication number
- CN101721840A CN101721840A CN200910201212A CN200910201212A CN101721840A CN 101721840 A CN101721840 A CN 101721840A CN 200910201212 A CN200910201212 A CN 200910201212A CN 200910201212 A CN200910201212 A CN 200910201212A CN 101721840 A CN101721840 A CN 101721840A
- Authority
- CN
- China
- Prior art keywords
- chromatographic column
- magnetic
- column
- filling
- magnetic fillers
- 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
Images
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention relates to a device and a method for preparing a chromatographic column made of a magnetic filling material. In the preparation method, magnetic materials or magnetic materials with a shell-core structure are used as a substrate of a chromatographic fixed phase to prepare the chromatographic fixed phase by surface modification, and the chromatographic fixed phase can be used for separation of a capillary electrochromatography, a liquid phase chromatography or a gas phase chromatography; for the filling materials with a bigger grain size, the pneumatic and slurry pole assembling methods and other pole assembling methods are adopted to complete the pole assembly, and an electromagnetic gun device designed in the invention is further used for tamping; and for the fixed phase with the smaller grain size or nanometer grain size, the electric filling method is used for filling, and the electromagnetic gun device is further used for tamping. The invention has the advantages that: the filling device is convenient in use, simple in structure and easy to configure and operate; and the chromatographic column fixed phase of the magnetic filling materials prepared by the method is uniform and dense and has a high chromatographic column efficiency.
Description
[technical field]
The present invention relates to the chromatographic column technical field, specifically, is a kind of preparation facilities and preparation method of magnetic fillers chromatographic column.
[background technology]
Along with proteomics research deepens continuously, magnetic material has obtained using widely in the research of gathering trace protein and peptide section.Magnetic material mainly is meant by transition element iron, and cobalt, nickel extremely alloy etc. can directly or indirectly produce the material of magnetic.Shell nuclear magnetism material is meant that mainly it is that the insulation shell is (as SiO that the composite Nano magnetic material with core/shell structure has outer shell concurrently
2, Al
2O
3, C-SiO
2Deng) or semiconductor shell (as ZnO etc.) composite and kernel be magnetic material because its structure and form and can on the nm nanoscale, design and cut out, thereby have the physics and the chemical property such as light, electricity, magnetic, catalysis of many uniquenesses.Compare with traditional phosphated peptide section enrichment material, magnetic material has remarkable advantages.It can make the destination protein that needs to separate be able to quick and easy separation in containing the first sample preparation product of solid suspension, keep the complete of target molecule to greatest extent, protein loss is few, to low-abundance protein, extremely acid and utmost point basonuclin, small molecular protein are all responsive.Therefore magnetic material reaches with Fe at present
3O
4For the magnetic metal oxide nanoparticle core-shell material of core has obtained extensive utilization and develop rapidly in enriching phosphated peptide section.Therefore, adopt magnetic material or shell nuclear magnetism material, become the chromatographic stationary phase by prepared by surface modification, can the egg collection white matter be detected on one with separating, very wide application prospect is arranged with the enrichment of peptide section according to the separation demand as chromatographic stationary phase matrix.
At present, the preparation method of chromatographic column mainly contains following several: capillary electric chromatographic column: homogenate method, pulling method and electronic completion method; Liquid-phase chromatographic column: dry method filling and wet method filling, i.e. homogenate method; Gas chromatographic column: pneumatic process.
The homogenate method: the organic solvent of filler and certain volume is mixed into equal homogenate, the capillary (stainless steel tube) of under pressure filler being packed into, this method advantage be simple to operate, the equipment requirement is low; But,, be difficult for filling because back-pressure is big for granule filler or long chromatographic column.Pulling method: be that silica gel is encased in the capillary of large diameter, under high temperature it be stretched to required internal diameter with the glass tensilometer, the advantage of this method is no stopper, removes the influence of stopper from; But uniformity is difficult to control during drawing by high temperature, and can destroy the binding groups of filler.Electronic completion method: be a kind ofly to replace high-pressure pump, add high voltage, utilize fixing electrophoretic force mutually itself to load, in the filling process, can come control device speed by the height of regulating high tension voltage at the capillary column two ends with high voltage source.The advantage of this method is to fill comparatively evenly, once can fill out many, owing to there is not back-pressure, can fill longer chromatographic column.Dry column-packing: be applicable to the liquid-phase chromatographic column filling of the filling of gas chromatographic column and packing material size greater than 20 μ m.Make the filler chromatographic column of under the air pressure effect, advancing to pack into by Pneumatic methods such as pressurization or decompression methods, perhaps make filler enter chromatographic column by the vibration or the method for beaing.But for the filler of small particle diameter,, assemble seriously between particle, be difficult to take on evenly and closely post bed because of the increasing of electrostatic interaction and surface energy.
And above method is all not very good for the filling of magnetic fillers, for the magnetic material of small particle diameter especially magnetic Nano material, uses the homogenate method to have the back-pressure height, the shortcoming that is difficult to load.Use pneumatic process, i.e. dry column-packing, magnetic material is easy to again reunite, and is difficult to evenly post bed closely of formation.The method that electricity consumption is filled is because the repulsive interaction between particles of magnetic material can't evenly be piled up the particle that enters in the chromatographic column closely.
[summary of the invention]
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation facilities and preparation method of magnetic fillers chromatographic column is provided.
Of the present invention being contemplated that: mainly adopt pneumatic process and homogenate method that it is filled in liquid phase or the gas chromatographic column in advance for big (5～10 μ m) magnetic of particle diameter or core-shell magnetic filler, utilize magnetic artillery dress column device of the present invention with the magnetic material compacting then, thereby make fixing evenly tight mutually.For particle diameter less (1～3 μ m) even nano-scale magnetic or core-shell structure magnetic material, mainly adopt homogenate method and electronic completion method that it is filled in the capillary electric chromatographic column in advance, utilize magnetic artillery dress column device of the present invention with the chromatographic column compacting then.Filling device is easy to use, and is simple in structure, is easy to configuration and operation; The chromatographic column of the magnetic fillers of preparation is fixing mutually even, fine and close, the chromatogram column efficiency height.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation facilities of magnetic fillers chromatographic column is the magnetic artillery device, is the electromagnetic circuit system of an electromagnetic induction, by power supply, and power switch, rectifier bridge, electric capacity, coil and holding circuit are formed, as Fig. 1.
Primary clustering and specifications parameter are as follows:
Power supply: 220V exchanges;
Power switch: maximum current-carrying 15～30A;
The maximum current-carrying 15～20A of four crystal diodes of rectifier bridge: D1～D4;
Electric capacity: parallel connection or series capacitance are some; Capacitance voltage 350～2000V; Electric capacity total capacity: 800～4000uF;
Coil: enamel covered wire, line footpath size 0.14～0.8mm, the number of turn 500～3000 circles; Hollow is used to place column jecket;
Holding circuit: 220V, the bulb assembly of 40～100W is some, or adopts fusible link;
Electronic devices and components are assembled into the electromagnetic circuit system of electromagnetic induction according to Fig. 2: power supply → holding circuit → rectifier bridge → electric capacity → power switch → coil;
A kind of preparation method of magnetic fillers chromatographic column, its concrete steps are:
One, filler modified and column jecket is handled
(1) separating property as required carries out modification by the hydrolysis-polymerisation of silica gel to the core-shell magnetic material surface; Can obtain C18, NH respectively
2, surface bond functional group such as CN separating medium, can be applied to different clastotypes such as reverse-phase chromatography, ion-exchange chromatography respectively;
(2) to select internal diameter for use be 4～6mm to performance liquid chromatographic column, and length is the stainless steel column jecket of 150～250mm; It is 25～150 μ m that capillary electric chromatographic column is selected internal diameter for use, and length is the capillary of 10～40cm;
(3) for the filling of performance liquid chromatographic column, before filling, must be to inside pipe wall strict cleaning the in addition; The step of cleaning is with the situation of general employing μ m level filler, the stainless steel column jecket is taken out with the hot NaOH aqueous solution and is washed 4～5 times, and with oil stain and the dirt of removing inside pipe wall, the water flushing is to neutral, at last with organic solvents such as acetone, ether flushing 2～3 times, dry for standby;
(4) for the filling of capillary electric chromatographic column, before filling, must carry out chemical treatment to inner surface; By chemical activation, activation process is that capillary column was washed 10～60 minutes with diluted acid, diluted alkaline successively, washes with water to neutrality according to general wherein capillary tube inner wall surface; Getting mass concentration is that 15% hydrofluoric acid charges into capillary, leaves standstill 0.5～1.5h after the sealing two ends, washes with water to neutrality, and nitrogen or air blow drying are standby;
Described diluted acid is selected from hydrochloric acid, a kind of in sulfuric acid or the nitric acid, and wherein, concentration of hydrochloric acid is 0.1mol/L; Sulfuric acid concentration is 0.1mol/L; Concentration of nitric acid is 0.1mol/L;
Described diluted alkaline is selected from a kind of in sodium hydroxide solution or the potassium hydroxide solution, and concentration of sodium hydroxide solution is 1mol/L; Potassium hydroxide solution concentration is 1mol/L;
(5) column cap of performance liquid chromatographic column must add sieve plate before filling, is retained in the post to guarantee filler, forms stable bed; Sieve plate is stainless steel or macromolecular material, sieve plate size and column jecket internal diameter coupling, and the aperture of sieve plate is at 10～500nm;
(6) electric chromatographic column must burn stopper near column cap before filling, was retained in the post to guarantee filler, formed stable bed;
Two, the preparation of magnetic fillers chromatographic column:
(1) magnetic fillers is filled in advance:
Chromatographic column is glass or macromolecule material, and column cap installs sieve plate in advance, and this stopper only allows gas and filling liquid freely to pass through, and magnetic fillers can't pass through;
For particle diameter is the magnetic fillers of 5～20 μ m, adopts dress column methods such as pneumatic, homogenate to finish pre-filling; Pneumatic process or homogenate method: the utilization high-pressure pump provides the pressure of 10～40MPa, and magnetic fillers is pre-loaded into chromatographic column;
For particle diameter is the magnetic fillers of 3nm～5 μ m or nano-scale, adopts electronic completion method to finish pre-filling; Electronic completion method is to utilize 0～30KV high voltage source to replace high-pressure pump, adds high voltage at the capillary column two ends, utilizes EOF and fixing mutually electrophoretic force own to carry out prefill;
(2) preparation of magnetic fillers chromatographic column: 1. the chromatographic column that is pre-charged with is inserted in the coil → 2. magnetic artillery dress column device inserts the electric current of 220V alternating current → 3. by capacitor C capacitance voltage: the 350～2000V of the rectifier bridge D1～D4 effect AC-DC of holding circuit assembly 220V 40～100W → 4. → 5.; Electric capacity total capacity: 800～4000uF is in the charging of the charged state → 6. electric current of the capacitor discharge of deenergization → 7. closed power supply plug-in strip K → 8. → 9. that finishes and flows through coil and produce high-intensity magnetic field; Magnetic material will be done ejection type and move in chromatographic column this moment, and the final whole chromatographic column of compacting obtains the chromatographic stationary phase of even compact, repeats above flow operations 2～15 times, each operating time, 2～7 seconds at interval; As shown in Figure 3, electric current I flows through coil, produces powerful magnetic field in the gc column tube, and magnetic direction points to N from S, magnetic fillers in the chromatographic column begins to do forward sling movement as the fixing effect that is subjected to powerful electromagnetic field mutually, and the most whole chromatographic column padding and compacting; Obtain the magnetic fillers chromatographic column.
Compared with prior art, good effect of the present invention is:
Magnetic fillers filling device of the present invention is easy to use, simple in structure, is easy to configuration and operation; The chromatographic column of the magnetic fillers of preparation is fixing mutually even, fine and close, the chromatogram column efficiency height.
[description of drawings]
Fig. 1 magnetic artillery device schematic diagram;
Fig. 2 magnetic artillery dress column device circuit diagram;
Fig. 3 magnetic artillery device loads schematic diagram to magnetic fillers.
[specific embodiment]
The preparation facilities of a kind of magnetic fillers chromatographic column of the present invention and preparation method's the specific embodiment below are provided.
Embodiment 1
300mg SBF-Fe
3O
4-SiO
2-NH
2The core-shell magnetic material adds 1mL methyl alcohol, ultrasonic 10min, the method that electricity the is filled capillary column of packing into.The chromatographic column of filling is in advance put into enamel-cover copper magnet wire circle (1000 circle) → access 220V to be exchanged, this interchange (is selected 450V for use through rectifier bridge direct current that becomes 450V that boosts to electric capacity charging → capacitor C, 990uF) charging finishes, 220V power supply → closed power switch K → the capacitor C of breaking (is selected 450V for use, 990uF) discharge → electric current is through enamel covered wire circle (radius 0.15mm, the number of turn 1000 circles) in chromatographic column, produce the magnetic or the shell nuclear magnetism filler of filling in advance in strong magnetic field → chromatographic column and be subjected to strong external magnetic field effect generation accelerated motion, launch the picture other end by chromatographic column one end.1. repeat above-mentioned capacitor charge and discharge process 10 times, each 3 seconds time intervals; 2. treat that the coil cooling repeats 1. to operate.Observe to find that through experiment in 10 minutes pre-magnetic of filling or core-shell structure magnetic filler be by initial dispersity, become density of texture fixing phase matrix uniformly.
Magnetic fillers filling device of the present invention is easy to use, simple in structure, is easy to configuration and operation; The chromatographic column of the magnetic fillers of preparation is fixing mutually even, fine and close, the chromatogram column efficiency height.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.
Claims (6)
1. the preparation facilities of a magnetic fillers chromatographic column; it is characterized in that; it is the magnetic artillery device; by power supply; power switch, rectifier bridge, electric capacity; coil and holding circuit are formed, and electronic devices and components are assembled into the electromagnetic circuit system of electromagnetic induction: power supply → holding circuit → rectifier bridge → electric capacity → power switch → coil.
2. the preparation facilities of a kind of magnetic fillers chromatographic column as claimed in claim 1 is characterized in that, described magnetic artillery device assembly and specifications parameter are as follows:
Power supply: 220V exchanges;
Power switch: maximum current-carrying 15～30A;
The maximum current-carrying 15～20A of four crystal diodes of rectifier bridge: D1～D4;
Electric capacity: parallel connection or series capacitance are some; Capacitance voltage 350～2000V; Electric capacity total capacity: 800～4000uF;
Coil: enamel covered wire, line footpath size 0.14～0.8mm, the number of turn 500～3000 circles; Hollow is used to place column jecket;
Holding circuit: 220V, the bulb assembly of 40～100W is some, or adopts fusible link.
3. the preparation method of a magnetic fillers chromatographic column is characterized in that, concrete steps are:
(1) magnetic fillers is filled in advance:
Chromatographic column is glass or macromolecule material, and column cap installs sieve plate in advance, and this stopper only allows gas and filling liquid freely to pass through, and magnetic fillers can't pass through;
For particle diameter is the magnetic fillers of 5～20 μ m, adopts pneumatic, homogenate dress column method to finish pre-filling;
For particle diameter is the magnetic fillers of 3nm～5 μ m or nano-scale, adopts electronic completion method to finish pre-filling;
(2) preparation of magnetic fillers chromatographic column: 1. the chromatographic column that is pre-charged with is inserted in the coil → 2. magnetic artillery dress column device inserts the electric current of 220V alternating current → 3. by capacitor C capacitance voltage: the 350～2000V of the rectifier bridge D1～D4 effect AC-DC of holding circuit assembly 220V 40～100W → 4. → 5.; Electric capacity total capacity: 800～4000uF is in the charging of the charged state → 6. electric current of the capacitor discharge of deenergization → 7. closed power supply plug-in strip K → 8. → 9. that finishes and flows through coil and produce high-intensity magnetic field; Magnetic material will be done ejection type and move in chromatographic column this moment, and the final whole chromatographic column of compacting obtains the chromatographic stationary phase of even compact, repeats above flow operations 2～15 times, each operating time, 2～7 seconds at interval; Electric current I flows through coil, produces powerful magnetic field in the gc column tube, and magnetic direction points to N from S, and the magnetic fillers in the chromatographic column begins to do forward sling movement as the fixing effect that is subjected to powerful electromagnetic field mutually, and the most whole chromatographic column padding and compacting; Obtain the magnetic fillers chromatographic column.
4. the preparation method of a kind of magnetic fillers chromatographic column as claimed in claim 3 is characterized in that, described pneumatic process or homogenate method: the utilization high-pressure pump provides the pressure of 10～40MPa, and magnetic fillers is pre-loaded into chromatographic column.
5. the preparation method of a kind of magnetic fillers chromatographic column as claimed in claim 3, it is characterized in that, described electronic completion method is to utilize 0～30KV high voltage source to replace high-pressure pump, adds high voltage at the capillary column two ends, utilizes EOF and fixing mutually electrophoretic force own to carry out prefill.
6. a magnetic fillers chromatographic column is in gas-chromatography, liquid chromatogram and capillary electric chromatogram Application for Field.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910201212A CN101721840A (en) | 2009-12-16 | 2009-12-16 | Device and method for preparing chromatographic column made of magnetic filling material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910201212A CN101721840A (en) | 2009-12-16 | 2009-12-16 | Device and method for preparing chromatographic column made of magnetic filling material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101721840A true CN101721840A (en) | 2010-06-09 |
Family
ID=42443759
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910201212A Pending CN101721840A (en) | 2009-12-16 | 2009-12-16 | Device and method for preparing chromatographic column made of magnetic filling material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101721840A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102338785A (en) * | 2010-07-16 | 2012-02-01 | 华东理工大学 | Preparation method of dynamic magnet-coated nano-sized solid-phase open-tubular capillary electric chromatography column |
| CN102680618A (en) * | 2011-03-09 | 2012-09-19 | 北京康华源医药信息咨询有限公司 | Column chromatographic analysis detection opening and closing technology and application thereof |
| CN103018380A (en) * | 2012-11-27 | 2013-04-03 | 张勇 | Voltage-adjustable directly-heated type chromatographic column |
| CN109001343A (en) * | 2018-10-10 | 2018-12-14 | 李素媛 | The device and method of the high performance liquid chromatography detection of protein in a kind of milk powder |
| CN113117380A (en) * | 2019-12-31 | 2021-07-16 | 江苏汉邦科技有限公司 | Novel chromatographic column and unloading method |
| CN115078602A (en) * | 2022-05-30 | 2022-09-20 | 郑州大学第一附属医院 | Capillary high-pressure liquid chromatographic column and ultrasonic preparation method and application thereof |
| CN115078602B (en) * | 2022-05-30 | 2024-05-28 | 郑州大学第一附属医院 | Capillary high-pressure liquid chromatographic column and ultrasonic preparation method and application thereof |
-
2009
- 2009-12-16 CN CN200910201212A patent/CN101721840A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102338785A (en) * | 2010-07-16 | 2012-02-01 | 华东理工大学 | Preparation method of dynamic magnet-coated nano-sized solid-phase open-tubular capillary electric chromatography column |
| CN102338785B (en) * | 2010-07-16 | 2013-07-10 | 华东理工大学 | Preparation method of dynamic magnet-coated nano-sized solid-phase open-tubular capillary electric chromatography column |
| CN102680618A (en) * | 2011-03-09 | 2012-09-19 | 北京康华源医药信息咨询有限公司 | Column chromatographic analysis detection opening and closing technology and application thereof |
| CN102680618B (en) * | 2011-03-09 | 2016-06-29 | 常州博闻迪医药科技有限公司 | A kind of column chromatography analysis detection switching technique and application thereof |
| CN103018380A (en) * | 2012-11-27 | 2013-04-03 | 张勇 | Voltage-adjustable directly-heated type chromatographic column |
| CN109001343A (en) * | 2018-10-10 | 2018-12-14 | 李素媛 | The device and method of the high performance liquid chromatography detection of protein in a kind of milk powder |
| CN113117380A (en) * | 2019-12-31 | 2021-07-16 | 江苏汉邦科技有限公司 | Novel chromatographic column and unloading method |
| CN115078602A (en) * | 2022-05-30 | 2022-09-20 | 郑州大学第一附属医院 | Capillary high-pressure liquid chromatographic column and ultrasonic preparation method and application thereof |
| CN115078602B (en) * | 2022-05-30 | 2024-05-28 | 郑州大学第一附属医院 | Capillary high-pressure liquid chromatographic column and ultrasonic preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101721840A (en) | Device and method for preparing chromatographic column made of magnetic filling material | |
| CN104028391B (en) | Magnetic rotation flow separation method and magnetic rotation stream separator | |
| CN103248338B (en) | A kind of circuits for triggering of reverse switch transistor | |
| CN105585728B (en) | A kind of method of carbon nanotube coated polymer microballoon | |
| CN101212128B (en) | Corona discharge device and particle charging device utilizing the corona discharge device | |
| CN106026334B (en) | Super capacitor three stage charging system circuit and its method for super capacitor fast charging | |
| CN201168647Y (en) | Dipolar charge electrostatic coagulation dust removing apparatus | |
| CN103665278A (en) | Core-shell type magnetic composite microsphere for separation and purification of recombinant proteins and preparation method thereof | |
| CN207998746U (en) | A kind of non-woven material tow sides electrostatic electret device simultaneously | |
| CN202570373U (en) | Ultrasonic atomization electric-grid dust removing plant | |
| CN106921148A (en) | A kind of direct current on-off device based on LC in parallel | |
| CN105498967A (en) | Novel dust precharged type electrostatically-enhanced granular-bed high-temperature dust removal system | |
| CN201158706Y (en) | Super-fine powder electrostatic feeding device for laser cladding | |
| CN101869829B (en) | Preparation method of carbon-titanium dioxide chromatography stationary phase with shell-core structure and application | |
| CN101759256B (en) | Filter device | |
| CN204093574U (en) | Novel pipe micro mist electrostatic precipitator | |
| CN103754857A (en) | Method for efficiently extracting monometallic endohedral fullerene M@C82 | |
| CN107170955A (en) | A kind of lithium ion battery that can conveniently disassemble recovery, preparation method and disassemble recovery method | |
| CN111253915A (en) | Phase-change microcapsule and preparation method and application thereof | |
| Zhang et al. | Fabrication of high-quality microcapsules containing ionic liquid for application in self-healing conductive materials | |
| CN203155404U (en) | Magnetic vortex separator | |
| CN2724842Y (en) | Magnetic dressing column | |
| CN106684334B (en) | A kind of preparation method of three-dimensional netted titanium dioxide/silicon composite | |
| CN110026137B (en) | Preparation method and application of three-dimensional porous algae-based/chitosan aerogel for uranium-containing wastewater treatment | |
| CN207338144U (en) | A kind of super capacitor that can conveniently disassemble recycling |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| AD01 | Patent right deemed abandoned |
Effective date of abandoning: 20100609 |
|
| C20 | Patent right or utility model deemed to be abandoned or is abandoned |