CN110508030A - A kind of Magnetic solid phases extraction column and its application method - Google Patents
A kind of Magnetic solid phases extraction column and its application method Download PDFInfo
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- CN110508030A CN110508030A CN201910882092.3A CN201910882092A CN110508030A CN 110508030 A CN110508030 A CN 110508030A CN 201910882092 A CN201910882092 A CN 201910882092A CN 110508030 A CN110508030 A CN 110508030A
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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
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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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
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/38—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving specific interaction not covered by one or more of groups B01D15/265 - B01D15/36
- B01D15/3861—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving specific interaction not covered by one or more of groups B01D15/265 - B01D15/36 using an external stimulus
- B01D15/3885—Using electrical or magnetic means
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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
- B01D15/42—Selective adsorption, e.g. chromatography characterised by the development mode, e.g. by displacement or by elution
- B01D15/424—Elution mode
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Abstract
The invention discloses a kind of Magnetic solid phases extraction column and its application methods.Magnetic solid phases extraction column of the invention, magnetic adsorbent is filled between two panels sieve plate, and the lower sieve plate is magnetic sieve plate；Magnetic material is utilized to be easily manipulated, convenient, flexible feature, after interacting with target analytes, since magnetic force is adsorbed to, lower floor lever of sieve tray stacks to form magnetic material cylinder magnetic material, cause the interaction repeatedly layer by layer collided of the target analytes when sample liquid flows through magnetic material cylinder with magnetic material by the second wheel, the probability that sample liquid is adsorbed is greatly improved, improves and isolates and purifies effect；For the sample liquid containing trace target analytes, the rate of recovery can be improved；The interaction time can be effectively reduced while improving adsorption recovery rate, improve efficiency.Meanwhile the formation and dispersion of magnetic material cylinder can be realized by control external force or magnetic force, flexible operation.
Description
Technical field
The present invention relates to technical field of biological chemistry detection, more particularly to a kind of Magnetic solid phases extraction column and its use
Method.
Background technique
During detection and analysis, since the composition of most of samples is more complex, and the content of target analytes is lower, no
It can be directly used in instrument analysis, sample must effectively be handled before detection, separate and be enriched with target analytes.But sample
Preprocessing process is generally all cumbersome, easily receives matrix interference, and take a long time, and seriously affects the efficiency and reliability of detection.
Therefore, efficiently enrichment target analytes are most important, are the committed steps during entire test and analyze.Solid Phase Extraction
(SPE) technology is a kind of sample pretreatment based on liquid-phase chromatographic analysis mechanism developed rapidly in recent years, have it is simple,
Efficiently, it with automation and few organic solvent consumption the advantages that, is widely used in and tests and analyzes in work.
In recent years, some analysis workers start to carry out sample pretreatment with Magnetic solid phases extraction (MSPE) technology, and take
Good application effect was obtained, it is avoided, and common solid phase extraction techniques are cumbersome to be crossed the easy blocking of column operation, adsorption column, repeat
The problems such as property is poor, thus have a good application prospect.In Magnetic solid phases extraction process, magnetic adsorbent is not directly filled into
It in adsorption column, and is added in sample solution, the target analytes in sample solution is adsorbed onto the magnetic absorption of dispersion
Agent surface recycles externally-applied magnetic field to separate the magnetic adsorbent for having adsorbed target analytes from matrix, finally by mesh
Mark object analyte desorption can reach the purpose of separation and concentration target analytes.
But present inventor has found that above-mentioned technology at least exists such as during realizing the embodiment of the present application
Lower technical problem: during separation and concentration, since adsorption must be via target analytes and magnetic adsorbent surface base
The mutual collision generation of group, therefore do not caught and probability with certain sample.It, can be by prolonging in high concentration object sample
The long interaction time improves the modes such as magnetic adsorbent concentration and carries out, but when for trace object sample, the rate of recovery is usual
It is difficult to ensure.
Summary of the invention
In order to make up the defect of prior art, the present invention provides a kind of Magnetic solid phases extraction column and its application method.
The technical problems to be solved by the invention are achieved by the following technical programs:
A kind of Magnetic solid phases extraction column, including column tube, the column tube are internally provided with upper sieve plate and lower sieve plate, two panels sieve plate it
Between be filled with magnetic adsorbent, the lower sieve plate is magnetic sieve plate.
Further, the magnetic sieve plate is made of permanent-magnet materials or non-permanent-magnet materials.
Further, the permanent-magnet materials include alnico, siderochrome cobalt, permanent-magnet ferrite, in rare earth material at least
It is a kind of；The non-permanent-magnet materials includes at least one of dilval, ferrocobalt, ferroaluminium, ferriferous oxide.
Further, the lower end of the column tube is equipped with liquid outlet, is provided with closing device on the liquid outlet.
Further, the closing device is valve or plug.
Further, the lower sieve plate has sieve pore, and the aperture of the sieve pore is less than the size of the magnetic adsorbent.
Further, the aperture of the sieve pore of the lower sieve plate be 0.1-800 μm, the lower sieve plate with a thickness of 1nm-1cm；
The size of the magnetic adsorbent is 1nm-1mm.
The present invention also provides the application methods of above-mentioned Magnetic solid phases extraction column, include the following steps:
S1. Magnetic solid phases extraction column is provided, the Magnetic solid phases extraction column includes column tube, and the column tube is internally provided with sieve
Plate and lower sieve plate, magnetic adsorbent is filled between two panels sieve plate, and the lower sieve plate is magnetic sieve plate；The lower end of the column tube is set
There is liquid outlet, is provided with closing device on the liquid outlet；
S2. the closing device is closed, the sample liquid containing target analytes, vortex mixed is added in Xiang Suoshu column tube；
S3. cylinder is formed in lower floor lever of sieve tray in magnetic fields magnetic adsorbent；
S4. the closing device is opened, sample liquid is made to flow through the closing device, the magnetic of target analytes has been adsorbed and inhaled
Attached dose；
S5. the magnetic adsorbent for having adsorbed target analytes is eluted, obtains prepare liquid.
Further, in the step S1, the assemble method of the Magnetic solid phases extraction column are as follows: close the column tube lower end
The closing device being arranged on liquid outlet is successively packed into lower sieve plate, magnetic absorption agent dispersing liquid and upper sieve plate into column tube；Open institute
State closing device, drained the magnetic absorption agent dispersing liquid using negative pressure so that magnetic adsorbent be filled in two panels sieve plate it
Between.
Further, in the step S1, the assemble method of the Magnetic solid phases extraction column are as follows: be successively packed into column tube
Lower sieve plate, magnetic adsorbent powder and upper sieve plate, so that magnetic adsorbent is filled between two panels sieve plate.
Further, the height of column is less than the distance between described two panels sieve plate.
Further, the magnetic sieve plate is made of non-permanent-magnet materials, and in step S3, column tube is placed in coil
The heart, the end line of the coil are in series with DC power supply, are powered so that the coil generates magnetic field.
Further, the magnetic sieve plate is made of permanent-magnet materials, in step S3, generates magnetic by the magnetic sieve plate
.
Further, in step S3, the column tube is made to be in plumbness.
The invention has the following beneficial effects:
Magnetic solid phases extraction column of the invention, magnetic adsorbent is filled between two panels sieve plate, and the lower sieve plate is magnetic sieve plate；
Magnetic material is utilized to be easily manipulated, convenient, flexible feature, after interacting with target analytes, magnetic material is due to magnetic
Power is adsorbed to lower floor lever of sieve tray and stacks to form magnetic material cylinder, and target analytes is caused to flow through magnetic material column in sample liquid
The probability that sample liquid is adsorbed is greatly improved by the interaction of the second wheel repeatedly collided layer by layer with magnetic material when body,
It improves and isolates and purifies effect；For the sample liquid containing trace target analytes, the rate of recovery can be improved；It is adsorbed back improving
The interaction time can be effectively reduced while yield, improve efficiency.Meanwhile the formation and dispersion of magnetic material cylinder can be with
It is realized by control external force or magnetic force, flexible operation.The separative efficiency of magnetic material cylinder cylinder can pass through external magnetic field
Intensity adjustment is suitble to the regulation of different separation requirements.
Specific embodiment
In a first aspect, the present invention provides a kind of Magnetic solid phases extraction column, including column tube, the column tube is internally provided with
Sieve plate and lower sieve plate, magnetic adsorbent is filled between two panels sieve plate, and the lower sieve plate is magnetic sieve plate.
Specifically, the upper sieve plate and the lower sieve plate are arranged from top to bottom in the column tube, and the upper sieve plate and
Magnetic adsorbent is filled between the lower sieve plate.
In the present invention, the type of magnetic adsorbent is not especially limited, can be adopted according to the difference of target analytes
With Magnetic solid phases extract in common various magnetic adsorbents, structure and preparation method reason all can pass through for this technology personnel
Technical manual is learnt or is known by routine experiment method.As an example, the magnetic adsorbent can be methacrylic acid table
The magnetic-particle of face modification can illegally be added with malachite green, the rhodamine B etc. in adsorption sample liquid；The magnetic adsorbent
Or the magnetic-particle of silica surface modification, it can also be inhaled with macromoleculars such as DNA, albumen in adsorption sample liquid
The antibiotic such as attached chloramphenicol.
In the present invention, the upper sieve plate can be Magnetic screen plate, or common non magnetic sieve in solid-phase extraction column
Plate, such as polyethylene sieve plate.
In the present invention, the magnetism sieve plate is made of permanent-magnet materials or non-permanent-magnet materials.
The permanent-magnet materials includes at least one of alnico, siderochrome cobalt, permanent-magnet ferrite, rare earth material, more excellent
Selection of land, the permanent-magnet materials are neodymium iron boron；But not limited to this, be also possible to other it is unlisted in the present embodiment but by
Other materials well-known to those skilled in the art.
The non-permanent-magnet materials includes at least one of dilval, ferrocobalt, ferroaluminium, ferriferous oxide；
But not limited to this, be also possible to other it is unlisted in the present embodiment but by other materials well-known to those skilled in the art
Material.
In the present invention, the preparation method of magnetic sieve plate is not especially limited, it can be using existing each in the prior art
The preparation method of the magnetic sieve plate of kind.
As a further improvement, the magnetism sieve plate is prepared by non-permanent-magnet materials and high molecular material, the system
Preparation Method is method one or method two or method three；
The method one is specifically includes the following steps: (1) is magnetic micro- as raw material preparation using non-permanent-magnet materials and high molecular material
Ball；(2) magnetic microsphere accumulation is placed in porous metal matrix filter plate center, is pressed using press.
In the present invention, the method and step and principle for preparing magnetic microsphere are all that this technology personnel can be obtained by technical manual
Know or known by routine experiment method, those skilled in the art can be using the preparation of existing magnetic microsphere in the prior art
Method, preferably, preparing the concrete operations of magnetic microsphere using non-permanent-magnet materials and high molecular material as raw material are as follows: (1) with
Non- permanent-magnet materials is that raw material prepares magnetic bead；(2) magnetic bead is added in the reaction system of high molecular material, preparation synthesis
Magnetic microsphere.
Wherein, the method and step and principle for preparing magnetic bead are all that this technology personnel can be learnt or be passed through by technical manual
Routine experiment method knows that those skilled in the art can be using the preparation method of existing magnetic bead in the prior art.With it is non-forever
For magnetic material is ferroso-ferric oxide, the concrete operations of magnetic bead are prepared are as follows: distinguish Iron trichloride hexahydrate and four water frerrous chlorides
It mixes, is vortexed uniform after being dissolved with ultrapure water；It is poured into the mixed liquor of ultrapure water and ammonium hydroxide, stirs, washing is into after reaction
Property, obtain ferroso-ferric oxide magnetic bead.
The concrete operations of the step (2) are as follows: the magnetic bead is mixed with styrene, polyvinylpyrrolidone, water, is taken out true
Empty letting nitrogen in and deoxidizing；Benzoyl Oxide is added after stablizing in stirring heating, temperature, reacts；Magnet washing, which is collected, obtains magnetic polyphenyl second
Alkene microballoon.
In method one in the present invention, magnetic microsphere accumulation is creatively placed in porous metal matrix filter plate center, is made
It is pressed with press, the aperture of obtained magnetic sieve plate is small, and magnetism is evenly distributed.
In the present invention, the method two is specifically includes the following steps: (1) provides the sintering being prepared by high molecular material
Sieve plate；(2) the magnetic bead dispersion liquid being prepared by non-permanent-magnet materials is provided；(3) by the sintering sieve plate and the magnetic bead point
Dispersion liquid mixing, back flow reaction, drying obtain the magnetic sieve plate.
Wherein, the preparation method of sintering sieve plate is not especially limited in the present invention, principle and preparation method are ability
Known to field technique personnel, as an example, it is described sintering sieve plate the preparation method comprises the following steps: by high molecular material put into mold in, will
Mold is placed in hot press, and compression moulding obtains sintering sieve plate.
Wherein, the high molecular material can be polyethylene powder, but not limited to this, it is also possible to other preparation sintering sieves
The common high molecular material of plate.
In step (2), it is that magnetic bead is prepared by non-permanent-magnet materials, then magnetic bead is dispersed in ethanol water, is formed
Magnetic bead dispersion liquid.
In method two of the invention, sintering sieve plate is first creatively prepared by high molecular material, then glues magnetic-particle
It is attached on sintering sieve plate, the aperture of obtained magnetic sieve plate is small, and magnetism is evenly distributed.
In the present invention, the method three is specifically includes the following steps: (1) with non-permanent-magnet materials and high molecular material is original
Material prepares magnetic microsphere；(2) magnetic microsphere is placed in metal die, metal die is placed in hot press, be pressed into
Type obtains the magnetic sieve plate.
Wherein, the method and step and principle for preparing magnetic microsphere be all this technology personnel can be learnt by technical manual or
Known by routine experiment method, those skilled in the art can be using the preparation side of existing magnetic microsphere in the prior art
Method, preferably, preparing the concrete operations of magnetic microsphere using non-permanent-magnet materials and high molecular material as raw material are as follows: (1) with non-
Permanent-magnet materials is that raw material prepares magnetic bead；(2) magnetic bead is added in the reaction system of high molecular material, preparation synthesis magnetic
Property microballoon.Wherein, the method and step and principle for preparing magnetic bead are all that this technology personnel can be learnt or be passed through by technical manual
Routine experiment method knows that those skilled in the art can be using the preparation method of existing magnetic bead in the prior art.With it is non-forever
For magnetic material is ferroso-ferric oxide, the concrete operations of magnetic bead are prepared are as follows: distinguish Iron trichloride hexahydrate and four water frerrous chlorides
It mixes, is vortexed uniform after being dissolved with ultrapure water；It is poured into the mixed liquor of ultrapure water and ammonium hydroxide, stirs, washing is into after reaction
Property, obtain ferroso-ferric oxide magnetic bead.
The concrete operations of the step (2) are as follows: the magnetic bead is mixed with styrene, polyvinylpyrrolidone, water, is taken out true
Empty letting nitrogen in and deoxidizing；Benzoyl Oxide is added after stablizing in stirring heating, temperature, reacts；Magnet washing, which is collected, obtains magnetic polyphenyl second
Alkene microballoon.
In the present invention, the size of metal die is not especially limited, those skilled in the art can be according to actual needs
It is set, as an example, the size of the metal die is 20*20*0.1cm.
The design parameter of hot press work is not especially limited in the present invention, those skilled in the art can be according to reality
It is set.
In method three in the present invention, magnetic microsphere is prepared using non-permanent-magnet materials and high molecular material as raw material, then will
The magnetic microsphere is placed in metal die, and metal die is placed in hot press, and compression moulding obtains the magnetic sieve plate, institute
The aperture of magnetism sieve plate obtained is small, and magnetism is evenly distributed.
In the present invention, the lower end of the column tube is equipped with liquid outlet, is provided with closing device on the liquid outlet.
The closing device can be valve, or plug, but not limited to this, it is also possible to other structures, only
Want can to control the opening and closing of liquid outlet.
In the present invention, the lower sieve plate has sieve pore, and the aperture of the sieve pore is less than the size of the magnetic adsorbent；Institute
State the sieve pore of lower sieve plate aperture be 0.1-800 μm, the lower sieve plate with a thickness of 1nm-1cm；The ruler of the magnetic adsorbent
Very little is 1nm-1mm.
In the present invention, aperture, the thickness etc. of the sieve pore of upper sieve plate are not especially limited, those skilled in the art can root
It is set according to actual needs.
Magnetic solid phases extraction column of the invention, magnetic adsorbent is filled between two panels sieve plate, and the lower sieve plate is magnetism
Sieve plate；Magnetic material is utilized to be easily manipulated, convenient, flexible feature, after interacting with target analytes, magnetic material
It stacks to form magnetic material cylinder since magnetic force is adsorbed to lower floor lever of sieve tray, target analytes is caused to flow through magnetism in sample liquid
Greatly improve what sample liquid was adsorbed by the interaction of the second wheel repeatedly collided layer by layer with magnetic material when material cylinder
Probability improves and isolates and purifies effect；For the sample liquid containing trace target analytes, the rate of recovery can be improved；It is improving
The interaction time can be effectively reduced while adsorption recovery rate, improve efficiency.Meanwhile the formation of magnetic material cylinder and point
Dissipating can be realized by control external force or magnetic force, flexible operation.The separative efficiency of magnetic material cylinder cylinder can be by outer
Magnetic field strength adjusting is set, the regulation of different separation requirements is suitble to.
Second aspect, the present invention also provides the application methods of above-mentioned Magnetic solid phases extraction column, include the following steps:
S1. Magnetic solid phases extraction column is provided, the Magnetic solid phases extraction column includes column tube, and the column tube is internally provided with sieve
Plate and lower sieve plate, magnetic adsorbent is filled between two panels sieve plate, and the lower sieve plate is magnetic sieve plate；The lower end of the column tube is set
There is liquid outlet, is provided with closing device on the liquid outlet；
S2. the closing device is closed, the sample liquid containing target analytes, vortex mixed is added in Xiang Suoshu column tube；
S3. cylinder is formed in lower floor lever of sieve tray in magnetic fields magnetic adsorbent；
S4. the closing device is opened, sample liquid is made to flow through the closing device, the magnetic of target analytes has been adsorbed and inhaled
Attached dose；
S5. the magnetic adsorbent for having adsorbed target analytes is eluted, obtains prepare liquid.
Wherein, in the step S1, the assemble method of the Magnetic solid phases extraction column can be with are as follows: closes the column tube lower end
The closing device being arranged on liquid outlet is successively packed into lower sieve plate, magnetic absorption agent dispersing liquid and upper sieve plate into column tube；Open institute
State closing device, drained the magnetic absorption agent dispersing liquid using negative pressure so that magnetic adsorbent be filled in two panels sieve plate it
Between.
In the step S1, the assemble method of the Magnetic solid phases extraction column can be with are as follows: under being successively packed into column tube
Sieve plate, magnetic adsorbent powder and upper sieve plate, so that magnetic adsorbent is filled between two panels sieve plate.
In the present invention, the state of column tube in step S2 is not especially limited, can be horizontality, it can also be with any
Angle tilt is placed, as long as splashing out sample liquid not.
It should be noted that in order to enable sample liquid does not splash out when vortex mixed, before vortex mixed, by column tube upper end cover
Tightly.
In the present invention, the state of column tube described in step S3 is not particularly limited, preferably, making the column tube can be with
In plumbness, the effect being arranged in this way is: magnetic adsorbent is easy since gravity declines on lower sieve plate naturally
Cylinder is formed by subsequent magnetic aggregation.
When the magnetic sieve plate is made of non-permanent-magnet materials, in step S3, column tube is placed in hub of a spool, the line
The end line of circle is in series with DC power supply, is powered so that the coil generates magnetic field；When the magnetic sieve plate is by permanent-magnet materials system
At in step S3, by the magnetic sieve plate generation magnetic field.
Solid-phase extraction column in the prior art can be compressed solid phase extraction adsorbents by two sieve plates, Solid Phase Extraction absorption
The height of agent is equal to the distance between sieve plate, and two sieve plates directly contact filler, then carries out analysis sample in column using mobile phase
Column chromatography on son is isolated and purified.But above-mentioned solid phase extraction column is very low to particle tolerance, carries out column in analysis sample
In chromatography process, it is necessary to which the phenomenon that removing very clean to particle, otherwise will cause stifled column leads to the failure of an experiment.Therefore
It is frequently necessary to carry out high speed centrifugation in use, the operation such as filtering is relatively complicated；Above-mentioned solid phase extraction column is in the process of filling
In, it needs for filler to be accurately placed in small sized pipeline, and applying certain pressure makes sieve plate compress solid phase extraction adsorbents.This gives
Production brings certain difficulty, for the solid phase extraction adsorbents of relatively low amount, in process of production, often due to pressure
Power is not constant enough, and causes solid phase extraction adsorbents density inconsistent, the situation that column tomographic results reproducibility is not good enough；And it is lesser
Pipeline, which loads production, also proposed higher equipment requirement.
In the present invention, the height of column is less than the distance between described two panels sieve plate.In this way, sample liquid can extract
Turbulent flow is formed in column, so that solid-phase extraction column greatly improves the tolerance of particle, and sample pre-treatments are greatly lowered
Difficulty, process effectively prevent the appearance of clogging, effectively increase the working efficiency of Solid Phase Extraction；Meanwhile it being filled out in filling
During material, upper sieve plate can control splint position by height, reduce pressure sensing difficulty without pressing to filler surface,
The problem for reducing because pressure unevenness causes density different, and then causing experimental result repeatability not good enough.
The present invention will now be described in detail with reference to examples, and the examples are only preferred embodiments of the present invention,
It is not limitation of the invention.
Embodiment 1
A kind of application method of Magnetic solid phases extraction column, includes the following steps:
S1. the column tube that capacity is 1ml is provided, the lower end of the column tube is equipped with liquid outlet, is provided with valve on the liquid outlet；It closes
Close the valve being arranged on the liquid outlet of the column tube lower end, be successively packed into column tube lower sieve plate, magnetic absorption agent dispersing liquid and on
Sieve plate；The valve is opened, is drained the magnetic absorption agent dispersing liquid using negative pressure, so that magnetic adsorbent is filled in two panels
Between sieve plate；Wherein, the upper sieve plate is polyethylene sieve plate, and the lower sieve plate is magnetic sieve plate, and the magnetism sieve plate is by neodymium iron
Boron is made；The distance between the upper sieve plate and lower sieve plate are 1cm；The volume of the magnetic absorption agent dispersing liquid is 0.6ml,
In the magnetic-particle containing 30mg methacrylic acid surface modification；
S2. the valve is closed, the sample liquid that 1ml contains target analytes is added in Xiang Suoshu column tube, column tube upper end is covered tightly,
Vortex mixed；
S3. so that the column tube is in plumbness, form cylinder in lower floor lever of sieve tray in magnetic fields magnetic adsorbent；It is described
Height of column is less than the distance between described two panels sieve plate；
S4. the valve is opened, sample liquid is made to flow through the valve, has been adsorbed the magnetic adsorbent of target analytes；
S5. the magnetic adsorbent for having adsorbed target analytes is eluted, obtains prepare liquid.
Embodiment 2
A kind of application method of Magnetic solid phases extraction column, includes the following steps:
S1. the column tube that capacity is 3ml is provided, the lower end of the column tube is equipped with liquid outlet, is provided with valve on the liquid outlet；It closes
Close the valve being arranged on the liquid outlet of the column tube lower end, be successively packed into column tube lower sieve plate, magnetic absorption agent dispersing liquid and on
Sieve plate；The valve is opened, is drained the magnetic absorption agent dispersing liquid using negative pressure, so that magnetic adsorbent is filled in two panels
Between sieve plate；Wherein, the upper sieve plate is polyethylene sieve plate, and the lower sieve plate is magnetic sieve plate, and the magnetism sieve plate is by poly- second
Alkene and ferroso-ferric oxide are made；The distance between the upper sieve plate and lower sieve plate are 2cm；The body of the magnetic absorption agent dispersing liquid
Product is 3ml, wherein the magnetic-particle containing the modification of 120mg silica surface；
S2. the valve is closed, the sample liquid that 2ml contains target analytes is added in Xiang Suoshu column tube, column tube upper end is covered tightly,
Vortex mixed；
S3. so that the column tube is in plumbness, column tube is placed in hub of a spool, the end line of the coil is in series with direct current
Source is powered so that the coil generates magnetic field, in magnetic fields magnetic adsorbent in lower floor lever of sieve tray formation cylinder；The column
Body height is less than the distance between described two panels sieve plate；
S4. the valve is opened, sample liquid is made to flow through the valve, has been adsorbed the magnetic adsorbent of target analytes；
S5. the magnetic adsorbent for having adsorbed target analytes is eluted, obtains prepare liquid.
Comparative example 1
Based on embodiment 1, the difference is that only: the lower sieve plate is polyethylene sieve plate.
Comparative example 2
Based on embodiment 1, the difference is that only: being filled in this comparative example 2 is non magnetic adsorbent between two panels sieve plate.
Comparative example 3
Using traditional Magnetic solid phases abstraction technique, magnetic adsorbent is not directly filled into column tube, and is added to and contains
Have in the sample liquid of target analytes, vortex mixed, the target analytes in sample liquid are adsorbed onto the magnetic adsorbent of dispersion
Surface recycles externally-applied magnetic field to separate the magnetic adsorbent for having adsorbed target analytes from matrix, finally by target
Object analyte desorption.
Test example
The preparation of sample liquid: taking 3 grams of chilli powder of mark-on 2ppm BaP, after pulverizer crushes again, is added and contains 5%DMSO
Acetonitrile solution 5mL, 1000rpm is centrifuged 1 minute, and the supernatant after then taking 1 milliliter of centrifugation and 2 milliliters of ultrapure waters mixings obtain
To sample liquid.1 milliliter of 1% formic acid methanol is added when elution.It is respectively adopted at embodiment 1 and the method for comparative example 1-3
Reason, record sample liquid flow completely out the time of lower end liquid outlet, and using the liquid chromatogram measuring rate of recovery, measurement result is referring to table 1.
* wherein comparative example 1-2 does not flow after 4 minutes because blocking, and is allowed to after being pressurizeed 7 minutes after 15 minutes using negative pressure
It reserves completely.
It can be seen that the Magnetic solid phases extraction column in the present invention, magnetic adsorbent is filled between two panels sieve plate, under described
Sieve plate is magnetic sieve plate, after interacting with target analytes, magnetic material lower floor lever of sieve tray heap since magnetic force is adsorbed to
It is folded to form magnetic material cylinder, it improves and isolates and purifies effect, for the sample liquid containing trace target analytes, can be improved
The rate of recovery.Be magnetic adsorbent or magnetic sieve plate are contained only in solid-phase extraction column, for the sample liquid containing trace target analytes,
It is difficult to ensure the rate of recovery.
Embodiments of the present invention above described embodiment only expresses, the description thereof is more specific and detailed, but can not
Therefore limitations on the scope of the patent of the present invention are interpreted as, as long as skill obtained in the form of equivalent substitutions or equivalent transformations
Art scheme should all be fallen within the scope and spirit of the invention.
Claims (10)
1. a kind of Magnetic solid phases extraction column, including column tube, the column tube is internally provided with upper sieve plate and lower sieve plate, and feature exists
In filled with magnetic adsorbent between two panels sieve plate, the lower sieve plate is magnetic sieve plate.
2. Magnetic solid phases extraction column as described in claim 1, which is characterized in that the magnetism sieve plate is by permanent-magnet materials or non-
Permanent-magnet materials is made；The permanent-magnet materials includes alnico, siderochrome cobalt, permanent-magnet ferrite, at least one in rare earth material
Kind；The non-permanent-magnet materials includes at least one of dilval, ferrocobalt, ferroaluminium, ferriferous oxide.
3. Magnetic solid phases extraction column as described in claim 1, which is characterized in that the lower end of the column tube is equipped with liquid outlet, institute
It states and is provided with closing device on liquid outlet.
4. Magnetic solid phases extraction column as described in claim 1, which is characterized in that the lower sieve plate has sieve pore, the sieve pore
Aperture be less than the magnetic adsorbent size；The aperture of the sieve pore of the lower sieve plate is 0.1-800 μm, the lower sieve plate
With a thickness of 1nm-1cm；The size of the magnetic adsorbent is 1nm-1mm.
5. a kind of application method of Magnetic solid phases extraction column, includes the following steps:
S1. Magnetic solid phases extraction column is provided, the Magnetic solid phases extraction column includes column tube, and the column tube is internally provided with sieve
Plate and lower sieve plate, magnetic adsorbent is filled between two panels sieve plate, and the lower sieve plate is magnetic sieve plate；The lower end of the column tube is set
There is liquid outlet, is provided with closing device on the liquid outlet；
S2. the closing device is closed, the sample liquid containing target analytes, vortex mixed is added in Xiang Suoshu column tube；
S3. cylinder is formed in lower floor lever of sieve tray in magnetic fields magnetic adsorbent；
S4. the closing device is opened, sample liquid is made to flow through the closing device, the magnetic of target analytes has been adsorbed and inhaled
Attached dose；
S5. the magnetic adsorbent for having adsorbed target analytes is eluted, obtains prepare liquid.
6. the application method of Magnetic solid phases extraction column as claimed in claim 5, which is characterized in that described in the step S1
The assemble method of Magnetic solid phases extraction column are as follows: the closing device being arranged on the liquid outlet of the column tube lower end is closed, successively to column tube
Sieve plate, magnetic absorption agent dispersing liquid and upper sieve plate under interior loading；The closing device is opened, the magnetic absorption agent dispersing liquid is taken out
It is dry, so that magnetic adsorbent is filled between two panels sieve plate.
7. the application method of Magnetic solid phases extraction column as claimed in claim 5, which is characterized in that described in the step S1
The assemble method of Magnetic solid phases extraction column are as follows: lower sieve plate, magnetic adsorbent powder and upper sieve plate are successively packed into column tube, so that
Magnetic adsorbent is filled between two panels sieve plate.
8. the application method of Magnetic solid phases extraction column as claimed in claim 5, which is characterized in that the height of column is less than institute
State the distance between two panels sieve plate.
9. the application method of Magnetic solid phases extraction column as claimed in claim 5, which is characterized in that it is described magnetism sieve plate by it is non-forever
Magnetic material is made, and in step S3, column tube is placed in hub of a spool, and the end line of the coil is in series with DC power supply, is powered
So that the coil generates magnetic field.
10. the application method of Magnetic solid phases extraction column as claimed in claim 5, which is characterized in that the magnetism sieve plate is by forever
Magnetic material is made, and in step S3, generates magnetic field by the magnetic sieve plate.
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