CN106749922B - A kind of preparation method and applications of beta-cyclodextrin hybridized polymer Microcolumn - Google Patents
A kind of preparation method and applications of beta-cyclodextrin hybridized polymer Microcolumn Download PDFInfo
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- CN106749922B CN106749922B CN201611049210.5A CN201611049210A CN106749922B CN 106749922 B CN106749922 B CN 106749922B CN 201611049210 A CN201611049210 A CN 201611049210A CN 106749922 B CN106749922 B CN 106749922B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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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
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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
- B01D15/265—Adsorption chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0009—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Glucans, e.g. polydextrose, alternan, glycogen; (alpha-1,4)(alpha-1,6)-D-Glucans; (alpha-1,3)(alpha-1,4)-D-Glucans, e.g. isolichenan or nigeran; (alpha-1,4)-D-Glucans; (alpha-1,3)-D-Glucans, e.g. pseudonigeran; Derivatives thereof
- C08B37/0012—Cyclodextrin [CD], e.g. cycle with 6 units (alpha), with 7 units (beta) and with 8 units (gamma), large-ring cyclodextrin or cycloamylose with 9 units or more; Derivatives thereof
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- 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
- G01N30/6052—Construction of the column body
Abstract
The invention discloses a kind of preparation method and applications of beta-cyclodextrin hybridized polymer Microcolumn, which synthesizes by the following method is made: (1) reacting beta-cyclodextrin with acryloyl chloride and acryloyl group-beta-cyclodextrin function monomer is made；(2) methanol is added in acryloyl group-beta-cyclodextrin function monomer and the bis- pore-foaming agents of DMF is uniformly mixed so as to obtain mixed liquor；(3) methyltrimethoxysilane, dressing agent 3- (isobutene acyl-oxygen) propyl trimethoxy silicane, crosslinking agent ethylene glycol dimethacrylate and initiator azodiisobutyronitrile is added; after vortex oscillation, ultrasonic treatment; liquid relief is in the liquid transfer gun head that one end seals; the silica gel sealing other end is used again; at 40~60 DEG C reaction 16~for 24 hours, obtain acryloyl group-beta-cyclodextrin hydridization Microcolumn.The present invention has synthesized a kind of novel solid phase microextraction adsorbing medium, can apply to the remaining detection of pesticide in food samples.
Description
Technical field
The present invention relates to a kind of solid phase micro-extraction technique fields, and in particular to a kind of beta-cyclodextrin hybridized polymer is integrally micro-
The preparation method and applications of column.
Background technique
Beta-cyclodextrin be by 7 D- glucopyranose units by Isosorbide-5-Nitrae-glucosides key connection at ring molecule, it is empty
Between structure in the shape of a spiral, molecule is in wide at the top and narrow at the bottom, both ends open, hollow tubular article, and intracavitary portion is in relative hydrophobicity, and is owned
For hydroxyl then outside molecule, this special molecular structure allows that beta-cyclodextrin is matched with many sizes and polarities match has
Machine molecule forms inclusion complex, so as to realize the molecular recognition to object, therefore, beta-cyclodextrin is optimized processing and is closed
It is applied to that there is biggish meaning in solid phase micro-extraction technique at novel separation adsorbent material.
Summary of the invention
Aiming at the problems existing in the prior art, the purpose of the present invention is to provide a kind of novel solid phase microextraction separation
The preparation method and applications of adsorbent material beta-cyclodextrin hybridized polymer Microcolumn.
To achieve the above object, the technical scheme adopted by the invention is as follows: a kind of beta-cyclodextrin hybridized polymer is integrally micro-
The preparation method of column, comprising the following steps: (1) beta-cyclodextrin is reacted with acryloyl chloride and acryloyl group-beta-cyclodextrin function is made
It can monomer；(2) methanol is added in acryloyl group-beta-cyclodextrin function monomer and the bis- pore-foaming agents of DMF is uniformly mixed so as to obtain mixed liquor；
(3) methyltrimethoxysilane, dressing agent 3- (isobutene acyl-oxygen) propyl trimethoxy silicon are added into the mixed liquor of step (2)
Alkane, crosslinking agent ethylene glycol dimethacrylate and initiator azodiisobutyronitrile are moved after vortex oscillation, ultrasonic treatment
Liquid is in the liquid transfer gun head that one end seals, then with the silica gel sealing other end, react 16 at 40~60 DEG C~for 24 hours, obtain propylene
Acyl-beta-cyclodextrin hydridization Microcolumn.
The beneficial effects of the present invention are: the present invention only uses acryloyl group-beta-cyclodextrin as function monomer, enhances poly-
The molecular recognition selectivity of object Microcolumn is closed, acryloyl group-beta-cyclodextrin function monomer and inorganic silicon Alkylators pass through friendship
Join the polymerization that agent occurs, hybrid inorganic-organic Microcolumn is prepared, both high with inorganic mechanical strength of silicon material,
The good advantage of absorption property, and the defect for overcoming organic polymer materials swelling, collapsing；With methanol and N,N-dimethylformamide
(DMF) it is double pore-foaming agents, increases the dissolubility of function monomer；The present invention is that synthesizing new separation is inhaled directly in liquid transfer gun head
Enclosure material can be combined with the syringe of various sizes, solid phase microextraction process be realized to facilitate, since beta-cyclodextrin is to pesticide
The Molecular Recognization that there is small organic molecule Subjective and Objective supermolecule to be formed, the hybridized polymer Microcolumn that the present invention is synthesized
Novel separation adsorbing medium as solid phase microextraction, may be implemented the separation and enrichment to pesticide small organic molecule, and separation is rich
Collect high-efficient, meanwhile, it is combined, pesticide residue can be carried out qualitative and quantitative with efficient liquid phase chromatographic analysis after solid phase microextraction
Analysis detection especially measures the analysis of organophosphorus pesticide, and high sensitivity, favorable reproducibility, the range of linearity are wide, detection limit is low.
Detailed description of the invention
Fig. 1 is that acryloyl group-beta-cyclodextrin hydridization Microcolumn of the present invention synthesizes schematic diagram；
Fig. 2 is the infared spectrum analyzed by infrared radiation instrument, wherein (a) be beta-cyclodextrin infrared line,
It (b) is that synthesize obtained infrared line, (c) of acryloyl group-beta-cyclodextrin be that acryloyl group-beta-cyclodextrin is miscellaneous to the present embodiment 1
Change the infrared line of Microcolumn；
Fig. 3 is that obtained acryloyl group-beta-cyclodextrin hydridization Microcolumn is synthesized to the present embodiment 1 by thermogravimetric analyzer
Obtained thermal decomposition figure；
Fig. 4 is the scanning electron microscope that the present embodiment 1 synthesizes obtained acryloyl group-beta-cyclodextrin hydridization Microcolumn.
Specific embodiment
The present invention will be described in detail combined with specific embodiments below, and the description of this part is only exemplary and explains
Property, there should not be any restriction effect to protection scope of the present invention.
A kind of preparation method of beta-cyclodextrin hybridized polymer Microcolumn of the invention, comprising the following steps:
(1) beta-cyclodextrin is reacted with acryloyl chloride and acryloyl group-beta-cyclodextrin function monomer is made；
(2) methanol is added in acryloyl group-beta-cyclodextrin function monomer and the bis- pore-foaming agents of DMF is uniformly mixed so as to obtain mixed liquor；
(3) methyltrimethoxysilane, dressing agent 3- (isobutene acyl-oxygen) propyl three are added into the mixed liquor of step (2)
Methoxy silane, crosslinking agent ethylene glycol dimethacrylate and initiator azodiisobutyronitrile, at vortex oscillation, ultrasound
After reason, liquid relief is in the liquid transfer gun head that one end seals, then with the silica gel sealing other end, react 16 at 40~60 DEG C~for 24 hours, it obtains
To acryloyl group-beta-cyclodextrin hydridization Microcolumn.
In above-mentioned technical proposal, the substance of the acryloyl group-beta-cyclodextrin function monomer and methyltrimethoxysilane
The ratio between amount be 1:4~5；The substance of the methyltrimethoxysilane and 3- (isobutene acyl-oxygen) propyl trimethoxy silicane
The ratio between amount is 2~3:1.
In above-mentioned technical proposal, in the step (1), the specific preparation process of acryloyl group-beta-cyclodextrin function monomer
It is as follows: to take beta-cyclodextrin, solvent DMF is added, add triethylamine, be ultrasonically treated 10~20min, then in ice-water bath slowly
The DMF solution of acryloyl chloride is added dropwise, after reacting 30~40min, moves to 30~40min of reaction under room temperature, stands, suction filtration removes
Concentrated by rotary evaporation filtrate after precipitating is gone, acetone is added and precipitating is precipitated, suction filtration is precipitated, and is dried in vacuo 12 at 80~90 DEG C
~for 24 hours, obtain acryloyl group-beta-cyclodextrin function monomer.
In above-mentioned technical proposal, the ratio between the beta-cyclodextrin, amount of substance of acryloyl chloride are 1:8.
In above-mentioned technical proposal, in the step (2), double pores will be added in acryloyl group-beta-cyclodextrin function monomer
Agent simultaneously stirs 0.5~1h at 40~60 DEG C.
In above-mentioned technical proposal, in the step (3), the methanol solution of nitric acid first is added simultaneously in methyltrimethoxysilane
After stirring 0.5~1h activation at 40~60 DEG C, activating solution is added in mixed liquor.
Shown in synthetic reaction process of the invention reaction equation (1) as shown in figure 1 and (2).
The present invention also provides a kind of application of beta-cyclodextrin hybridized polymer Microcolumn, the beta-cyclodextrin hydridization is poly-
It closes object Microcolumn and is used for food Detecting Pesticide.
Further, the beta-cyclodextrin hybridized polymer Microcolumn is for solid phase microextraction-high performance liquid chromatography connection
With the analysis measurement that in analysis determining technology, can be used in actual sample to pesticide residue.
The Monolithic Columns that the present invention synthesizes can carry out solid phase by the direct combination of liquid transfer gun head and syringe
Micro-extraction process, it is convenient, quick, which can be applied to consolidate pesticide small organic molecule in vegetables actual sample
Phase extraction separation and concentration, the analysis detection of Organic pesticide residues suitable for vegetables is subsequent to be combined again with high performance liquid chromatography,
Highly sensitive highly selective qualitative and quantitative analysis measurement can be able to achieve to organic agricultural chemicals, especially to organophosphorus pesticide.
Embodiment 1
A kind of specific synthetic method of beta-cyclodextrin hybridized polymer Microcolumn of the present embodiment is as follows: (1) acryloyl
The synthesis of group-beta-cyclodextrin function monomer: weighing 1mmol beta-cyclodextrin, and the DMF of 30mL, stirring and dissolving, then plus 1.17mL is added
Then the DMF solution of the good 8mmol acryloyl chloride of refrigerator cold-storage is slowly added dropwise in triethylamine, ultrasonic 10min in ice-water bath
1.5mL is moved to after reacting 30min and is reacted 30min under room temperature, is stood, and a large amount of precipitatings are precipitated, filter after removing precipitating, rotation
Inspissation contracting, then plus two volumes acetone, have a white precipitate precipitation, filter and simultaneously precipitated 2 times with a large amount of acetone washings, then 80 DEG C very
The dry 12h of sky, obtains acryloyl group-beta-cyclodextrin function monomer；(2) 0.1mmol acryloyl group-beta-cyclodextrin function monomer is taken
It is dissolved in 1mL pore-foaming agent, methanol 0.6mL and DMF 0.4mL mixed solvent is added and is uniformly mixed, is stirred under the conditions of 40 DEG C
30min；(3) 200 μ L and 0.4mmol methyltrimethoxysilane of the nitric acid solution mixing for taking 300 μ L of methanol, 0.1mol/L,
Activating solution is added in step (2) after stirring 1h activation under the conditions of 40 DEG C, the 3- (isobutyl of 0.2mmol is then added thereto
Alkene acyl-oxygen) propyl trimethoxy silicane, 150 μ L ethylene glycol dimethacrylates and 4.0mg azodiisobutyronitrile, by whirlpool
After oscillation, ultrasonic treatment 30min, liquid relief is in the liquid transfer gun head that one end seal, then with the silica gel sealing other end, at 40 DEG C instead
Acryloyl group-beta-cyclodextrin hydridization Microcolumn material should be obtained for 24 hours.
Embodiment 2
A kind of specific synthetic method of beta-cyclodextrin hybridized polymer Microcolumn of the present embodiment is as follows: (1) acryloyl
The synthesis of group-beta-cyclodextrin function monomer: weighing 1mmol beta-cyclodextrin, and the DMF of 30mL, stirring and dissolving, then plus 1.17mL is added
Then the DMF solution of the good 8mmol acryloyl chloride of refrigerator cold-storage is slowly added dropwise in triethylamine, ultrasonic 20min in ice-water bath
1.5mL is moved to after reacting 40min and is reacted 40min under room temperature, is stood, and a large amount of precipitatings are precipitated, filter after removing precipitating, rotation
Inspissation contracting, then plus two volumes acetone, have a white precipitate precipitation, filter and simultaneously precipitated 2 times with a large amount of acetone washings, then 90 DEG C very
The dry 12h of sky, obtains acryloyl group-beta-cyclodextrin function monomer；(2) 0.1mmol acryloyl group-beta-cyclodextrin function list is weighed
Body is dissolved in 1mL pore-foaming agent, and methanol 0.6mL and DMF 0.4mL mixed solvent is added and is uniformly mixed, stirs 1 under the conditions of 50 DEG C
Hour；(3) methyltrimethoxysilane of nitric acid solution 200 the μ L and 0.45mmol of 300 μ L of methanol, 0.1mol/L is taken to mix,
Activating solution is added in step (2) after stirring 30min activation under the conditions of 50 DEG C, the 3- of 0.15mmol is then added thereto
(isobutene acyl-oxygen) propyl trimethoxy silicane, 150 μ L ethylene glycol dimethacrylates and 4.0mg azodiisobutyronitrile, warp
After crossing vortex oscillation, ultrasonic treatment 30min, liquid relief is in the liquid transfer gun head that one end seals, then with the silica gel sealing other end, 50
18h is reacted at DEG C, obtains acryloyl group-beta-cyclodextrin hydridization Microcolumn material.
Embodiment 3
A kind of specific synthetic method of beta-cyclodextrin hybridized polymer Microcolumn of the present embodiment is as follows: (1) acryloyl
The synthesis of group-beta-cyclodextrin function monomer: weighing 1mmol beta-cyclodextrin, and the DMF of 30mL, stirring and dissolving, then plus 1.17mL is added
Then the DMF solution of the good 8mmol acryloyl chloride of refrigerator cold-storage is slowly added dropwise in triethylamine, ultrasonic 10min in ice-water bath
1.5mL is moved to after reacting 30min and is reacted 40min under room temperature, is stood, and a large amount of precipitatings are precipitated, filter after removing precipitating, rotation
Inspissation contracting, then plus two volumes acetone, have a white precipitate precipitation, filter and simultaneously precipitated 2 times with a large amount of acetone washings, then 80 DEG C very
Sky is dry for 24 hours, obtains acryloyl group-beta-cyclodextrin function monomer；(2) 0.1mmol acryloyl group-beta-cyclodextrin function list is weighed
Body is dissolved in 1mL pore-foaming agent, and methanol 0.6mL and DMF 0.4mL mixed solvent is added and is uniformly mixed, stirs under the conditions of 60 DEG C
30min；(3) methyltrimethoxysilane of nitric acid solution 200 the μ L and 0.5mmol of 300 μ L of methanol, 0.1mol/L is taken to mix,
Activating solution is added in step (2) after stirring 30min activation under the conditions of 60 DEG C, the 3- of 0.25mmol is then added thereto
(isobutene acyl-oxygen) propyl trimethoxy silicane, 150 μ L ethylene glycol dimethacrylates and 4.0mg azodiisobutyronitrile, warp
After crossing vortex oscillation, ultrasonic treatment 30min, liquid relief is in the liquid transfer gun head that one end seals, then with the silica gel sealing other end, 60
16h is reacted at DEG C, obtains acryloyl group-beta-cyclodextrin hydridization Microcolumn material.
1, infared spectrum is analyzed:
Fig. 2 is the infared spectrum analyzed by infrared radiation instrument, and it is this that (a), which is the infrared line of beta-cyclodextrin, (b),
Infrared line, (c) that embodiment 1 synthesizes obtained acryloyl group-beta-cyclodextrin are that acryloyl group-beta-cyclodextrin hydridization is integrally micro-
The infrared line of column；Also there is new absorption peak, 1735cm in the characteristic peak for remaining beta-cyclodextrin in (b) as seen from the figure-1
It is the characteristic absorption peak of C=O, 1636cm-1It is the characteristic absorption peak of C=C, 1205cm-1It is the absorption peak of (C=O)-O, then table
Bright acryloyl chloride has been successfully introduced into beta-cyclodextrin molecular structure；(c) characteristic absorption peak of C=C almost disappears in, and goes out
1271cm is showed-1、1135cm-1And 780cm-1Si-O-Si characteristic absorption peak, then show that acryloyl group-beta-cyclodextrin has been sent out
Raw hybrid polymer reaction, obtains hydridization Microcolumn material.
2, capability analysis is thermally decomposed:
Fig. 3 is that obtained acryloyl group-beta-cyclodextrin hydridization Microcolumn is synthesized to the present embodiment 1 by thermogravimetric analyzer
Obtained thermal decomposition figure, as seen from the figure, the Microcolumn material just start to decompose after 300 DEG C, show heat at normal temperature
It has good stability, is suitable for solid phase microextraction process.
3, electron-microscope scanning structural analysis:
Fig. 4 is the scanning electron microscope (SEM) photograph that the present embodiment 1 synthesizes obtained acryloyl group-beta-cyclodextrin hydridization Microcolumn, by
Figure is it is found that many of skeleton structure of Microcolumn material diameter is 1 μm or so of hole path, thus in target molecule
On the basis of being attracted on material, mobile phase can pass through the Microcolumn under lower back pressure, separation and concentration is high-efficient,
Sensitivity and selectivity are high.
The above is only presently preferred embodiments of the present invention, not makes any restrictions to technical scope of the invention, therefore
Any subtle modifications, equivalent variations and modifications to the above embodiments according to the technical essence of the invention, still belong to
In within the scope of technical solution of the present invention.
Claims (8)
1. a kind of preparation method of beta-cyclodextrin hybridized polymer Microcolumn, it is characterised in that: the following steps are included:
(1) beta-cyclodextrin is reacted with acryloyl chloride and acryloyl group-beta-cyclodextrin function monomer is made；
(2) methanol is added in acryloyl group-beta-cyclodextrin function monomer and the bis- pore-foaming agents of DMF is uniformly mixed so as to obtain mixed liquor；
(3) methyltrimethoxysilane, dressing agent 3- (isobutene acyl-oxygen) propyl trimethoxy are added into the mixed liquor of step (2)
Base silane, crosslinking agent ethylene glycol dimethacrylate and initiator azodiisobutyronitrile, by vortex oscillation, ultrasonic treatment
Afterwards, liquid relief is in the liquid transfer gun head that one end seals, then with the silica gel sealing other end, react 16 at 40~60 DEG C~for 24 hours, it obtains
Acryloyl group-beta-cyclodextrin hydridization Microcolumn.
2. the preparation method of beta-cyclodextrin hybridized polymer Microcolumn as described in claim 1, it is characterised in that: described third
The ratio between amount of substance of enoyl--beta-cyclodextrin function monomer and methyltrimethoxysilane is 1:4~5；The methyl trimethoxy
The ratio between oxysilane and the amount of substance of 3- (isobutene acyl-oxygen) propyl trimethoxy silicane are 2~3:1.
3. the preparation method of beta-cyclodextrin hybridized polymer Microcolumn as described in claim 1, it is characterised in that: the step
Suddenly in (1), the specific preparation process of acryloyl group-beta-cyclodextrin function monomer is as follows: beta-cyclodextrin is taken, solvent DMF is added, then
Triethylamine is added, is ultrasonically treated 10~20min, is then slowly added dropwise the DMF solution of acryloyl chloride in ice-water bath, reaction 30~
After 40min, 30~40min of reaction under room temperature is moved to, is stood, concentrated by rotary evaporation filtrate after removing precipitating is filtered, adds third
Ketone be precipitated precipitating, suction filtration precipitated, and at 80~90 DEG C vacuum drying 12~for 24 hours, obtain acryloyl group-beta-cyclodextrin function
It can monomer.
4. the preparation method of beta-cyclodextrin hybridized polymer Microcolumn as claimed in claim 3, it is characterised in that: the β-
The ratio between amount of substance of cyclodextrin, acryloyl chloride is 1:8.
5. the preparation method of beta-cyclodextrin hybridized polymer Microcolumn as described in claim 1, it is characterised in that: the step
Suddenly in (2), double pore-foaming agents will be added in acryloyl group-beta-cyclodextrin function monomer and stirs 0.5~1h at 40~60 DEG C.
6. the preparation method of beta-cyclodextrin hybridized polymer Microcolumn as described in claim 1, it is characterised in that: the step
Suddenly in (3), the methanol solution of nitric acid first is added in methyltrimethoxysilane and stirs 0.5~1h activation at 40~60 DEG C
Afterwards, activating solution is added in mixed liquor.
7. a kind of application of beta-cyclodextrin hybridized polymer Microcolumn, it is characterised in that: the preparation as described in claim 1~6
Obtained beta-cyclodextrin hybridized polymer Microcolumn is used for the detection of Pesticide Residues.
8. the application of beta-cyclodextrin hybridized polymer Microcolumn as claimed in claim 7, it is characterised in that: the β-ring paste
Smart hybridized polymer Microcolumn is for being used for food sample in solid phase microextraction-high performance liquid chromatography combination analysis determination techniques
The remaining analysis measurement of pesticide in product.
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| CN107286304A (en) * | 2017-07-06 | 2017-10-24 | 湖北大学 | Acryloyl group beta cyclodextrin POSS Fe3O4Magnetic particle is synthesized and applied |
| CN107597070B (en) * | 2017-10-30 | 2020-01-07 | 江南大学 | Hybrid adsorption material with hybrid silicon-cyclodextrin as core-shell structure and preparation method thereof |
| CN108722373B (en) * | 2018-06-25 | 2021-08-17 | 湖北大学 | Solid-phase microextraction fiber coating and preparation method and application thereof |
| CN109781899A (en) * | 2019-03-08 | 2019-05-21 | 无锡微色谱生物科技有限公司 | A method of using the screening of gas chromatography tandem mass spectrometry method and measurement green onion, ginger, 54 kinds of pesticide multi-residues in garlic |
| CN113736030A (en) * | 2020-05-30 | 2021-12-03 | 江苏大学 | High-frequency low-loss modified polyphenylene ether-based composite material |
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