CN109342626A - POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A and preparation method thereof - Google Patents
POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A and preparation method thereof Download PDFInfo
- Publication number
- CN109342626A CN109342626A CN201811435666.4A CN201811435666A CN109342626A CN 109342626 A CN109342626 A CN 109342626A CN 201811435666 A CN201811435666 A CN 201811435666A CN 109342626 A CN109342626 A CN 109342626A
- Authority
- CN
- China
- Prior art keywords
- ochratoxin
- specific recognition
- column
- inorganic hybrid
- hybrid molecule
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses POSS organic-inorganic hybrid molecule trace integral posts of specific recognition ochratoxin A and preparation method thereof, belong to analytical chemistry field.The integral post is using high hydrophilic organic polymerized monomer, crosslinking agent, template, initiator and binary pore-foaming agent as raw material, and dissolution forms uniform solution, and free radical thermal-initiated polymerization reaction occurs in injection column and is directly formed, after rinse through column to get finished product.The POSS organic-inorganic hybrid molecule trace integral post load capacity of prepared specific recognition ochratoxin A is big in the present invention, high specificity, stable mechanical performance, preparation method is simple and efficient, specific recognition suitable for ochratoxin A separates, the molecular engram integral column in beer matrix to the detection rate of recovery of ochratoxin A up to 96.6%, provide new way for the specific recognition separation of ochratoxin A.
Description
Technical field
The invention belongs to analytical chemistry fields, and in particular to the POSS organic and inorganic of specific recognition ochratoxin A is miscellaneous
Chemoattractant molecule trace integral post and preparation method thereof.
Background technique
Molecular engram integral column (Molecular Imprinted Monolithic Column, MIPMC) is to send out in recent years
Open up a kind of rapidly new chromatographic filler integral post.Its chromatograph packing material macroporous polymer medium is synthesized by in-situ polymerization
It is polymerize in empty tube column by monomer, initiator, crosslinking agent and porogen solutions and is made.Molecular engram integral column has preparation process
Simply, the advantages that mass transfer velocity is fast, reproducible, column forces down is a kind of chromatographic stationary phases very with application potential, thus
People are received more and more to pay attention to.Molecular engram integral column is divided into three classes according to the difference of preparation method and raw material: having
Machine molecularly imprinted polymer integral post, inorganic molecule trace integral post and organic-inorganic hybrid molecule trace integral post.Organic point
Sub- imprinted polymer integral post has the ready availability of outstanding pH stability and various monomers.However, when being exposed to different stream
When dynamic phase, these materials may contraction or expansion, and the different degrees of swelling in different solvents may significantly change
The form of polymer network；Inorganic molecule trace integral post has good optical property, mechanical performance and chemical inertness, but
The problems such as inorganic molecule trace integral post is inevitably present cracking and contraction, and sol-gel process is difficult to control.And
Organic-inorganic hybrid molecule trace integral post then can successfully overcome organic molecule trace integral post and inorganic molecule trace whole
The shortcomings that column.
Polyhedral oligomeric sesquialter silane (POSS) has unique cage structure, since it is easy to chemical modification, good
PH tolerance, high temperature resistant, it is anti-oxidant the advantages that, be used as function monomer or crosslinking agent to be widely used in hybrid integral material
Preparation.Since POSS is used to prepare molecular engram integral column for the first time by Li seminar, the imprinted material based on POSS is got over
Come more concerns (J Chromatogr A2015,1425,180-188).Utilize POSS monomer, especially vinyl POSS
It is the effective ways for improving gained imprinted polymer compatibility, simplifying preparation process.However, currently based on POSS trace integral post
Report it is also seldom, advantage is adequately proved not yet.In particular, there is presently no vinyl POSS hydridization integral posts
Binding molecule engram technology, one kettle way preparation have the report of specific recognition molecules trace integral post to ochratoxin A (OTA)
Road.
Summary of the invention
The purpose of the present invention is to provide the POSS organic-inorganic hybrid molecule traces of specific recognition ochratoxin A
Integral post and preparation method thereof.The integral post load capacity is big, high specificity, stable mechanical performance, and preparation method is simple and efficient.It is
By realizing high hydrophilic organic polymerized monomer, crosslinking agent, template, initiator and two using cause by way of " one-step polymerization "
The highly compatible of first five kinds of components of pore-foaming agent realizes quick, high efficiency, stabilization using free radical thermal-initiated polymerization reaction in column
Molecular engram integral column preparation, obtained molecular engram hydridization integral post can realize the efficient identification to object, and
To the rate of recovery of object in beer matrix up to 96.6%.
To achieve the above object, the present invention adopts the following technical scheme:
The POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A is to polymerize high hydrophilic organic
Monomer, crosslinking agent, template, initiator and binary pore-foaming agent are raw material, and dissolution forms uniform solution, inject in column and pass through generation
Free radical thermal-initiated polymerization and directly formed.
Above-mentioned high hydrophilic organic polymerized monomer are as follows: 2- acrylamide-2-methyl propane sulfonic monomer；Crosslinking agent are as follows: cage modle
Oligomeric sesquialter multi-polysiloxane and acrylate；Above-mentioned template is ochratoxin A solution；Above-mentioned initiator are as follows: azo
Two isobutyl cyanogen；Above-mentioned binary pore-foaming agent are as follows: N,N-dimethylformamide and PEG 10000；
Further, the mass ratio of above-mentioned polyhedral oligomeric sesquialter multi-polysiloxane and acrylate is 1:(20-25)；The binary
Pore-foaming agent, composition is by mass percentage are as follows: 10000 3.5%- of n,N-Dimethylformamide 93.5%-96.5%, PEG
6.5%；
Further, the polyhedral oligomeric sesquialter multi-polysiloxane is the polyhedral oligomeric sesquialter silicon that methacrylate connects branch
Oxygen alkane；The acrylate of stating is ethylene glycol dimethacrylate；
Further, the mass ratio of high hydrophilic organic polymerized monomer and crosslinking agent are as follows: 10.7: 85.3-14.7: 89.3；
Further, binary pore-foaming agent shared matter in high hydrophilic organic polymerized monomer, crosslinking agent and pore-foaming agent three's gross mass
Amount percentage is 75-83%；The dosage of template is both high hydrophilic organic polymerized monomer and crosslinking agents gross mass mass percent
25%-26%；Ochratoxin A concentration is 250-1000 ppb in template；The dosage of initiator is high hydrophilic organic polymerized monomer
With the 0.9%-1.1% of both crosslinking agents gross mass mass percent；
The preparation method of the POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A, including it is following
Step:
(1) quartz capillary column pre-processes: using 0.1 mol/L HCl to rinse 30 min respectively in vitreous silica capillary, with steaming
Distilled water is rinsed 30 minutes, is rinsed 3 hours with 0.1 mol/L NaOH, is rinsed 30 minutes with distilled water and methanol, then existed respectively
At room temperature with dry 30 min of 0.4 MPa nitrogen；In order to which C=C key is introduced capillary inner surface with bonding hybridization matrix, by body
γ-MAPS the methanol solution that product percentage is 50% injects in capillary, then capillary is placed on by both ends silicone rubber seal
24 h of heating water bath in 60 DEG C of water-bath；Later, 30 min of capillary is rinsed with methanol, then passes through 0.4 at 70 DEG C
Dry 30 min of MPa nitrogen are for further use；
(2) high hydrophilic organic polymerized monomer, crosslinking agent and initiator are added in centrifuge tube, then by binary pore-foaming agent and template
It is added into centrifuge tube, vortex oscillation 20-30 min, ultrasonic degassing 20-30 min form it into uniform solution at room temperature；
(3) by the solution quartz capillary column that injection step (1) has pre-processed at room temperature that step (2) obtains, both ends are close
It is honored as a queen and immerses 50-60 DEG C of water-bath successive reaction 10-15 h；The integral post prepared is taken out after the reaction was completed, is connected to liquid phase
Chromatographic solvent high-pressure pump washes away template and unreacted substance using methanol until pressure is stablized；
(4) buffer is passed through in integral post obtained by step (3), is saved at a temperature of 4 DEG C.
The composition of above-mentioned buffer are as follows: 10 mmol/L Tris-HCl, 120 mmol/L NaCl, 5 mmol/L KCl and
20 mmol/L CaCl2, pH 8.5.
The POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A of the present invention exists
Beer, grape wine, the application in juice drinks actual sample in the separation and enrichment of ochratoxin A ingredient.But the drink
Kind class is not limited only to the above type.
Remarkable advantage of the invention is:
(1) present invention, which combines POSS base integral post with molecular imprinting technology, is prepared for specific recognition ochratoxin A
POSS organic-inorganic hybrid molecule trace integral post；
(2) molecular engram integral column prepared by the present invention may be implemented to ochratoxin A specific isolation；
(3) molecular engram integral column prepared by the present invention is 5.9 ng(100 μm of i.d. × 10 to the ultimate load of OTA
Cm)；
(4) molecular engram integral column prepared by the present invention can be used in beer the efficiently concentrating of ochratoxin A with separate,
It detects the rate of recovery up to 96.6%.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of molecular engram integral column；It is 700 times left, it is 2000 times right.
Fig. 2 is the specific test of molecular engram integral column；A: column is compareed for non-molecular engram, b: for molecular engram entirety
Column；OTB: ochratoxin A；OTA: ochratoxin A.
Fig. 3 is the breakthrough curve figure of molecular engram integral column.
Fig. 4 is the mechanical stability of molecular engram integral column；Binding buffer solution: combination buffer；
MeOH: methanol；ACN: acetonitrile；H2O: water；Eluant solution: eluent.
Fig. 5 is specific test of the molecular engram integral column to ochratoxin A in beer.
Specific embodiment
Further to disclose rather than the present invention is limited, the present invention is made below in conjunction with specific embodiment further detailed
It describes in detail bright.
Embodiment 1
POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A and preparation method thereof is specific to walk
Suddenly are as follows:
(1) quartz capillary column pre-processes: using 0.1 mol/L HCl to rinse 30 min respectively in vitreous silica capillary, with steaming
Distilled water is rinsed 30 minutes, is rinsed 3 hours with 0.1 mol/L NaOH, is rinsed 30 minutes with distilled water and methanol, then existed respectively
At room temperature with dry 30 min of 0.4 MPa nitrogen stream；In order to which C=C key is introduced capillary inner surface with bonding hybridization matrix, incite somebody to action
γ-MAPS methanol (v/v) solution that percent by volume is 50% injects in capillary, both ends silicone rubber seal, then by capillary
Pipe is placed on 24 h of heating water bath in 60 DEG C of water-bath；Later, 30 min of capillary is rinsed with methanol, then led at 70 DEG C
It is for further use to cross dry 30 min of 0.4 MPa nitrogen；
(2) in mass ratio be 12.7: 3.8: 83.5 ratio, precise 2- acrylamide-2-methyl propane sulfonic monomer,
Methacrylate connects the polyhedral oligomeric silsesquioxane of branch and ethylene glycol dimethacrylate is added in centrifuge tube, quasi-
The dosage that initiator is really added accounts for the 1.0% of both monomer and crosslinking agent gross mass mass percent, accurate that binary pore-foaming agent is added
Amount be in high hydrophilic organic polymerized monomer, crosslinking agent and pore-foaming agent three's gross mass shared mass percent be 79%, successively
It is added into 2.0 mL centrifuge tubes, the dosage of template is then accounted for the 25.5% of both monomer and crosslinking agent gross mass percentage
Ochratoxin A concentration is that the template of 500 ppb is added into centrifuge tube, at room temperature 20 min of vortex oscillation, ultrasonic degassing 20
Min forms it into uniform solution；
(3) by the solution quartz capillary column that injection step (1) has pre-processed at room temperature that step (2) obtains, both ends are close
It is honored as a queen and immerses 55 DEG C of 12 h of water-bath successive reaction；The integral post prepared is taken out after the reaction was completed, it is molten to be connected to liquid chromatogram
Agent high-pressure pump washes away template and unreacted substance using methanol until pressure stabilization, can obtain column B；
(4) buffer is passed through in integral post obtained by step (3), is saved at a temperature of 4 DEG C.The composition of buffer are as follows: 10
Mmol/L Tris-HCl, 120 mmol/L NaCl, 5 mmol/L KCl and 20 mmol/L CaCl2, pH 8.5.
Embodiment 2
The template that ochratoxin A concentration is 250 ppb is added, other steps such as embodiment 1 can obtain column A.
Embodiment 3
The template that ochratoxin A concentration is 750 ppb is added, other steps such as embodiment 1 can obtain column C.
Embodiment 4
The template that ochratoxin A concentration is 1000 ppb is added, other steps such as embodiment 1 can obtain column D.
Embodiment 5
The amount of addition binary pore-foaming agent shared quality in high hydrophilic organic polymerized monomer, crosslinking agent and pore-foaming agent three's gross mass
Percentage is 75%, other steps such as embodiment 1 can obtain column E.
Embodiment 6
The amount of addition binary pore-foaming agent shared weight in high hydrophilic organic polymerized monomer, crosslinking agent and pore-foaming agent three's gross mass
Percentage is 83%, other steps such as embodiment 1 can obtain column F.
Embodiment 7
Addition is the 2- acrylamide-2-methyl propane sulfonic monomer of 14.7: 3.7: 81.6 ratio, methyl-prop in mass ratio
Olefin(e) acid ester connects the polyhedral oligomeric silsesquioxane and ethylene glycol dimethacrylate of branch, other steps such as embodiment 1 can obtain
Column G.
Embodiment 8
Addition is the 2- acrylamide-2-methyl propane sulfonic monomer of 10.7: 3.9: 85.5 ratio, methyl-prop in mass ratio
Olefin(e) acid ester connects the polyhedral oligomeric silsesquioxane and ethylene glycol dimethacrylate of branch, other steps such as embodiment 1 can obtain
Column H.
1 POSS hybrid inorganic-organic ochratoxin A molecular engram integral column preparation condition of table optimizes table
The specific test of 9 molecular engram integral column of embodiment
Column and 1 gained molecular engram integral column B of embodiment detection are compareed to the specificity of ochratoxin A using non-molecular engram
Identification.10 cm of column length is implemented according to the following steps respectively: (1) balancing: first being balanced 0.5 hour with combination buffer, chromatographic condition
For 0.10 mL/min of flow velocity, 250 psi of pressure, the combination buffer is 10 mmol/L Tris-HCl, 120 mmol/L
NaCl, 5 mmol/L KCl and 20 mmol/L CaCl2, pH 8.50；(2) it is enriched with: by final concentration of 10 ng/mL's of 20 μ L
Ochratoxin A (OTA) and final concentration of 100 ng/mL ochratoxin B(OTB) mixed solution be injected separately into two kinds of columns
In son, at whole on-column enrichment 1 hour, chromatographic condition was 0.02 mL/min, 250 psi of pressure；(3) it cleans: enriching column is filled
Onto liquid chromatography pump, control column and molecular engram integral column are respectively washed with combination buffer；Cleaning condition is flow velocity 0.1
ML/min, 250 psi of pressure, it is to be checked to collect last cleaning solution；(4) elute: using acetic acid: methanol=2: 98(v/v) as washing
De- liquid elutes ochratoxin A from integral post, and 250 psi backpressure valves, 0.1 mL/min of flow velocity collects washing for 20 μ L
De- liquid is to be checked.Using collection liquid is detected on HPLC- fluorescence detector, control column does not have specific recognition to ochratoxin A, and
Poor (Fig. 2 a) to ochratoxin A and ochratoxin B enrichment and elution effect, OTA in molecular engram integral column can be with
It is effectively recognized enrichment and elutes (Fig. 2 b).
The binding capacity of 10 molecular engram integral column of embodiment measures
With dynamic frontal method measurement ochratoxin A in specific recognition ochratoxin A prepared by the present invention
Breakthrough curve (breakthrough curve) in POSS organic-inorganic hybrid molecule trace integral post, and calculated with this whole
The maximal absorptive capacity of scapus.By the OTA solution of 50 ng/mL with the flow velocity of 0.02 mL/min by point of 10 cm effective column lengths
Sub- trace integral post is to calculate the integral post to the maximum load (Q of object OTAmax), receive and measure the stream of every 20 μ L
The peak area of OTA draws out breakthrough curve figure (Fig. 3) in liquid out.It was determined that the centre of maximum peak area from breakthrough curve
Corresponding volume (the V of pointR) it is 120 μ L, the in addition voidage (V of integral post0) can be according to formula V0=Vtotal-Vcapillary(its
In, Vtotal=μ×ttotal, μ indicates the flow velocity of mobile phase in capillary column, when t indicates that mobile phase passes through used in capillary column
Between, experiment select not retention toluene as marker) be calculated as V0=170 nL, according to formula Qmax=C(VR-V0) (C generation
The concentration (ng/mL) of table object OTA) molecular engram integral column is calculated is 5.9 ng to the ultimate load of OTA
(100 μm of cm of i.d. × 10).
The mechanical stability of 11 molecular engram integral column of embodiment measures
The POSS organic-inorganic hybrid molecule trace integral post of the specific recognition ochratoxin A prepared using embodiment 1 is set
In micro- liquid phase pump, in the mobile phase of five kinds of opposed polarities (methanol, water, ACN, eluent, combination buffer), flowed by changing
Relationship between its variation of speed measurement and integral post back pressure.As shown in figure 4, molecular engram integral column in five kinds of mobile phases, flows
Good linear dependence, R is presented with back pressure in speed2Reach 0.9927 ~ 0.99927, it is seen that molecular engram prepared by the present invention
Integral post has good mechanical stability.
Application Example 1
Molecular engram integral column in the embodiment 1 of use tests its bioaccumulation efficiency to ochratoxin A in beer.Pass through
Mark-on experiment, the ochratoxin A standard solution of 0.2 ng/mL is added in beer.OTA in practical beer sample can be with
It is effectively recognized and is enriched with and elutes (Fig. 5), the detection rate of recovery of the OTA in beer matrix is 96.6 ± 3.1%, 3 surveys
Fixed relative standard deviation is 3.0%.
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, is all covered by the present invention.
Claims (9)
1. the POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A, it is characterised in that: described
POSS organic-inorganic hybrid molecule trace integral post is with high hydrophilic organic polymerized monomer, crosslinking agent, template, initiator and binary
Pore-foaming agent is raw material, and dissolution forms uniform solution, and free radical thermal-initiated polymerization reaction occurs in injection column and is directly formed.
2. the POSS organic-inorganic hybrid molecule trace of specific recognition ochratoxin A according to claim 1 is whole
Column, it is characterised in that: the high hydrophilic organic polymerized monomer is 2- acrylamide-2-methyl propane sulfonic monomer；The crosslinking
Agent is polyhedral oligomeric sesquialter multi-polysiloxane and acrylate；The template is ochratoxin A solution；The initiator
For azo-bis-isobutyl cyanide；The binary pore-foaming agent is N,N-dimethylformamide and PEG 10000.
3. the POSS organic-inorganic hybrid molecule trace of specific recognition ochratoxin A according to claim 2 is whole
Column, it is characterised in that: the mass ratio of the polyhedral oligomeric sesquialter multi-polysiloxane and acrylate is 1:(20-25)；Described two
First pore-foaming agent, composition is by mass percentage are as follows: 10000 3.5%- of n,N-Dimethylformamide 93.5%-96.5%, PEG
6.5%。
4. the POSS organic-inorganic hybrid molecule trace of specific recognition ochratoxin A according to claim 2 is whole
Column, it is characterised in that: the polyhedral oligomeric sesquialter multi-polysiloxane is the polyhedral oligomeric sesquialter silicon that methacrylate connects branch
Oxygen alkane；The acrylate of stating is ethylene glycol dimethacrylate.
5. the POSS organic-inorganic hybrid molecule trace of specific recognition ochratoxin A according to claim 1 is whole
Column, it is characterised in that: the mass ratio of high hydrophilic organic polymerized monomer and crosslinking agent are as follows: 10.7: 85.3-14.7: 89.3.
6. the POSS organic-inorganic hybrid molecule trace of specific recognition ochratoxin A according to claim 1 is whole
Column, it is characterised in that: binary pore-foaming agent shared matter in high hydrophilic organic polymerized monomer, crosslinking agent and pore-foaming agent three's gross mass
Amount percentage is 75-83%；The dosage of template is both high hydrophilic organic polymerized monomer and crosslinking agents gross mass mass percent
25%-26%；Ochratoxin A concentration is 250-1000 ppb in template；The dosage of initiator is high hydrophilic organic polymerized monomer
With the 0.9%-1.1% of both crosslinking agents gross mass mass percent.
7. the POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A as described in claim 1
Preparation method, which comprises the following steps:
(1) quartz capillary column pre-processes: using 0.1 mol/L HCl to rinse 30 min respectively in vitreous silica capillary, then uses
It distilled water flushing 30 minutes, is rinsed 3 hours with 0.1 mol/L NaOH, rinses 30 minutes respectively with distilled water and methanol, then
At room temperature with dry 30 min of 0.4 MPa nitrogen；In order to which C=C key is introduced capillary inner surface with bonding hybridization matrix, incite somebody to action
Volume is that the γ-MAPS methanol solution of percentage 50% injects in capillary, then both ends silicone rubber seal is put capillary
24 h of heating water bath in 60 DEG C of water-bath；Later, 30 min of capillary is rinsed with methanol, then with 0.4 at 70 DEG C
Dry 30 min of MPa nitrogen are for further use；
(2) high hydrophilic organic polymerized monomer, crosslinking agent and initiator are added in centrifuge tube, then again by binary pore-foaming agent and
Template is added into centrifuge tube, at room temperature vortex oscillation 20-30 min, ultrasonic degassing 20-30 min, forms it into uniform molten
Liquid；
(3) by the solution quartz capillary column that injection step (1) has pre-processed at room temperature that step (2) obtains, both ends are close
It is honored as a queen and immerses 50-60 DEG C of water-bath successive reaction 10-15 h；The integral post prepared is taken out after the reaction was completed, is connected to liquid phase
Chromatographic solvent high-pressure pump washes away template and unreacted substance using methanol until pressure is stablized；
(4) buffer is passed through in integral post obtained by step (3), is saved at a temperature of 4 DEG C.
8. the POSS organic-inorganic hybrid molecule trace of specific recognition ochratoxin A according to claim 7 is whole
The preparation method of column, it is characterised in that: the composition of buffer described in step (4) are as follows: 10 mmol/L Tris-HCl, 120
Mmol/L NaCl, 5 mmol/L KCl and 20 mmol/L CaCl2, pH 8.5.
9. the POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A as described in claim 1
Application in beer, grape wine, juice drinks actual sample in the separation and enrichment of ochratoxin A ingredient.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811435666.4A CN109342626A (en) | 2018-11-28 | 2018-11-28 | POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811435666.4A CN109342626A (en) | 2018-11-28 | 2018-11-28 | POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109342626A true CN109342626A (en) | 2019-02-15 |
Family
ID=65318519
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811435666.4A Pending CN109342626A (en) | 2018-11-28 | 2018-11-28 | POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109342626A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110102270A (en) * | 2019-06-03 | 2019-08-09 | 福州大学 | A kind of affine integral post of aptamer of specific recognition F2 toxin and preparation method thereof |
| CN110605104A (en) * | 2019-08-08 | 2019-12-24 | 福州大学 | Aptamer-imprinted monolithic column for specifically recognizing ochratoxin A and preparation method thereof |
| CN113441120A (en) * | 2021-05-20 | 2021-09-28 | 河南工业大学 | Ochratoxin A metal organic framework NH2-MIL-53 molecularly imprinted material and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101308066A (en) * | 2008-06-12 | 2008-11-19 | 济南大学 | Trace amount mycotoxins molecular blotting column preparation method and application |
| US20100105076A1 (en) * | 2007-03-20 | 2010-04-29 | Polyintell | Analysis kit comprising at least two molecularly imprinted polymers and at least one marker, and method of analysis using same |
| CN102549424A (en) * | 2009-08-27 | 2012-07-04 | 全技术公司 | Synthetic mycotoxin adsorbents and methods of making and utilizing the same |
| CN102626609A (en) * | 2012-04-16 | 2012-08-08 | 福州大学 | Organic-inorganic hybrid protein molecular engram capillary tube monolithic column |
| CN106731005A (en) * | 2017-02-27 | 2017-05-31 | 福州大学 | A kind of organic polymer integral post of specific recognition ochratoxin and preparation method thereof |
| CN107118354A (en) * | 2017-05-24 | 2017-09-01 | 河南工业大学 | A kind of preparation method and application of the compound separating medium of ochratoxin metal organic framework molecular engram |
| CN107163226A (en) * | 2017-06-20 | 2017-09-15 | 吉林省爱诺德生物工程有限公司 | A kind of preparation method of Ochratoxin A molecularly imprinted polymer |
| CN108107144A (en) * | 2017-12-29 | 2018-06-01 | 福州大学 | A kind of POSS of aptamer functionalization is crosslinked organic-silica gel hybridization integral post and preparation method thereof |
-
2018
- 2018-11-28 CN CN201811435666.4A patent/CN109342626A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100105076A1 (en) * | 2007-03-20 | 2010-04-29 | Polyintell | Analysis kit comprising at least two molecularly imprinted polymers and at least one marker, and method of analysis using same |
| CN101308066A (en) * | 2008-06-12 | 2008-11-19 | 济南大学 | Trace amount mycotoxins molecular blotting column preparation method and application |
| CN102549424A (en) * | 2009-08-27 | 2012-07-04 | 全技术公司 | Synthetic mycotoxin adsorbents and methods of making and utilizing the same |
| US20120214897A1 (en) * | 2009-08-27 | 2012-08-23 | Alltech, Inc. | Synthetic mycotoxin adsorbents and methods of making and utilizing the same |
| CN102626609A (en) * | 2012-04-16 | 2012-08-08 | 福州大学 | Organic-inorganic hybrid protein molecular engram capillary tube monolithic column |
| CN106731005A (en) * | 2017-02-27 | 2017-05-31 | 福州大学 | A kind of organic polymer integral post of specific recognition ochratoxin and preparation method thereof |
| CN107118354A (en) * | 2017-05-24 | 2017-09-01 | 河南工业大学 | A kind of preparation method and application of the compound separating medium of ochratoxin metal organic framework molecular engram |
| CN107163226A (en) * | 2017-06-20 | 2017-09-15 | 吉林省爱诺德生物工程有限公司 | A kind of preparation method of Ochratoxin A molecularly imprinted polymer |
| CN108107144A (en) * | 2017-12-29 | 2018-06-01 | 福州大学 | A kind of POSS of aptamer functionalization is crosslinked organic-silica gel hybridization integral post and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| MINGHUO WU ET AL: "Polyhedral Oligomeric Silsesquioxane as a Cross-linker for Preparation of Inorganic−Organic Hybrid Monolithic Columns", 《ANAL. CHEM.》 * |
| YIQIONG CHEN ET AL: "Aptamer-based polyhedral oligomeric silsesquioxane (POSS)-containing hybrid affinity monolith prepared via a "one-pot" process for selective extraction of ochratoxin A", 《JOURNAL OF CHROMATOGRAPHY A》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110102270A (en) * | 2019-06-03 | 2019-08-09 | 福州大学 | A kind of affine integral post of aptamer of specific recognition F2 toxin and preparation method thereof |
| CN110102270B (en) * | 2019-06-03 | 2021-06-01 | 福州大学 | Aptamer affinity monolithic column for specifically recognizing F2 toxin and preparation method thereof |
| CN110605104A (en) * | 2019-08-08 | 2019-12-24 | 福州大学 | Aptamer-imprinted monolithic column for specifically recognizing ochratoxin A and preparation method thereof |
| CN113441120A (en) * | 2021-05-20 | 2021-09-28 | 河南工业大学 | Ochratoxin A metal organic framework NH2-MIL-53 molecularly imprinted material and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109342626A (en) | POSS organic-inorganic hybrid molecule trace integral post of specific recognition ochratoxin A and preparation method thereof | |
| CN108107144A (en) | A kind of POSS of aptamer functionalization is crosslinked organic-silica gel hybridization integral post and preparation method thereof | |
| CN102068968B (en) | Lead ion imprinting integral column and preparation method thereof | |
| CN107175053A (en) | A kind of preparation method of the covalent organic framework complex microsphere of core shell structure | |
| CN103920308B (en) | Polymer substrate capillary monolithic column that one is clicked based on Cu (I) and preparation method thereof | |
| CN106731005B (en) | A kind of organic polymer integral post of specific recognition ochratoxin and preparation method thereof | |
| CN105536293B (en) | A kind of affine organic silica gel hydridization integral post of boric acid and preparation method thereof | |
| CN110605104A (en) | Aptamer-imprinted monolithic column for specifically recognizing ochratoxin A and preparation method thereof | |
| CN112756016A (en) | Grafting type anion exchange resin chromatographic packing and preparation method thereof | |
| CN108211424A (en) | It is a kind of for POSS base organic-inorganic hybridisation silica gel integral posts of ochratoxin specific recognition and preparation method thereof | |
| CN110115992A (en) | A kind of aptamer functional poly zygostyle and preparation method thereof for mycotoxin specific recognition | |
| JP2002210377A (en) | Anion exchanger and its production method and application | |
| CN103881057A (en) | Preparation method for organic-inorganic hybrid porous monolith material based on epoxide ring-opening reaction | |
| CN107413320A (en) | A kind of application of protein A affinity chromatography medium | |
| CN106693931A (en) | Glucosamine oligosaccharide-functionalized hybrid silica monolithic column and preparation method | |
| CN104289209B (en) | A kind of WCX/HIC for Separation of Proteins difunctional mixed model polymeric matrix chromatographic stationary phases and preparation method thereof | |
| Zhao et al. | Towards highly specific aptamer-affinity monolithic column by efficient UV light-initiated polymerization in “one-pot” | |
| CN106977648B (en) | Method for preparing bisphenol A molecularly imprinted material from functional monomer containing template molecular structure | |
| CN109400823A (en) | Integral post and preparation method thereof that the boron of eight vinyl-POSS and ethylene glycol dimethacrylate co-crosslinking is affine | |
| CN110102270B (en) | Aptamer affinity monolithic column for specifically recognizing F2 toxin and preparation method thereof | |
| Adrian et al. | New analytical methods for epoxy resins, 2. Two‐dimensional chromatography | |
| CN112755592A (en) | Covalent organic framework nano microsphere functionalized solid phase microextraction monolithic column | |
| CN108187367B (en) | Sulfydryl derivatization L-PROLINE type organic-inorganic hybridization monolithic column and preparation method thereof | |
| CN104437438A (en) | Resin surface modified chromatographic packing, preparation method thereof and solid-phase extraction column | |
| CN102059157A (en) | Anion exchange integral material as well as conventional liquid phase chromatographic column or quartz capillary column taking anion exchange integral material as separating medium and preparation method thereof |
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 |
Application publication date: 20190215 |
|
| RJ01 | Rejection of invention patent application after publication |