A kind of phenylboronic acid-chitosan modified monolithic column and its preparation method and application
A technology of chitosan and phenylboronic acid, applied in chemical instruments and methods, other chemical processes, instruments, etc., can solve the problems of poor non-specific adsorption effect of monolithic columns, achieve high sensitivity and improve adsorption capacity
Active Publication Date: 2022-04-08
JIANGSU UNIV OF TECH
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Problems solved by technology
[0007] In order to solve the technical problem of poor non-specific adsorption effect of boric acid-modified monolithic columns, a phenylboronic acid-chitosan-modified monolithic column and its preparation method and application are provided
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Embodiment 1
[0036] A preparation method of a phenylboronic acid-chitosan modified monolithic column:
[0037] (1) Preparation of alkylated chitosan: 1 g of chitosan (deacetylation degree greater than 85%) was dissolved in 100 mL (v / v, 1%) of HAc solution, magnetically stirred until gelatinous and transferred to 250 mL In a three-necked flask, take 0.1mL of allyltrimethoxysilane in 15mL of absolute ethanol to form an allyltrimethoxysilanol solution, and slowly drop the allyltrimethoxysilanol solution into the gelatin-like shell In a 250mL three-necked flask of polysaccharide, react in a water bath at 60°C for 6h to prepare an alkylated chitosan solution;
[0038] (2) Preparation of phenylboronic acid functionalized chitosan: add 0.4mol / L NaOH solution 20mL in the alkylated chitosan solution that step (1) makes to carry out alkalization reaction until obtaining white flocculation precipitation, will obtain The precipitate was washed several times with ethanol and deionized water, and dried...
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The present invention relates to a monolithic column modified by phenylboronic acid-chitosan and its preparation method and application. The steps are as follows: react chitosan with allyltrimethoxysilane to prepare an alkylated chitosan solution into Drop into alkali solution and carry out alkalization precipitation reaction to obtain modified chitosan; Hydroxysuccinimide and the modified chitosan are stirred and reacted below 40°C to prepare phenylboronic acid functionalized chitosan; the prepared phenylboronic acid functionalized chitosan, methacrylic acid, ethylene glycol The dimethacrylate, alcohol and initiator are evenly mixed and then injected into the activated capillary, reacted at a temperature lower than 80°C, and a monolithic column modified with phenylboronic acid-chitosan is obtained after washing. It is used as solid phase microextraction material and combined with high performance liquid chromatography to detect nucleoside substances. The method of the invention has the effects of rapid detection of nucleosides and high sensitivity.
Description
technical field [0001] The invention relates to the technical field of monolithic column material preparation, in particular to a phenylboronic acid-chitosan modified monolithic column and its preparation method and application. Background technique [0002] With the advancement of science, the field of analytical chemistry has developed rapidly. For the separation of complex components, general enrichment materials can no longer meet the separation requirements. In recent years, monolithic column materials have been favored by researchers, and have been widely used in biology, medicine, agriculture and other fields due to their advantages such as simple preparation, fast analysis speed, and high mechanical strength. [0003] Chitosan (CS) is obtained by deacetylation of chitosan (Chitin), and it exists widely in nature. Various chemical reactions can occur under certain conditions, such as halogenation, nitration, redox, etc. Since Rouget first obtained chitosan in 1859,...
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IPC IPC(8): B01J20/24B01J20/281B01J20/30G01N30/02
CPCB01J20/24B01J20/22B01J20/281G01N30/02
Inventor 刘丹孙文杰陈栋东
Owner JIANGSU UNIV OF TECH