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Chitosan derivatization calix [4] arene bonded silica gel stationary phase and preparing method and application thereof

A technology for bonding silica gel and chitosan, which is applied in chemical instruments and methods, and other chemical processes, can solve the problems of failure to meet separation requirements, poor solubility of chitosan, and poor separation effect, and achieve improved bonding Quantity, improve hydrophilic performance, good separation selectivity effect

Active Publication Date: 2016-05-25
江苏国技仪器有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The researchers of the applicant unit had previously bonded chitosan (500Da) on the surface of silica gel to prepare a chromatographic column, but because of the poor solubility of chitosan and the low amount of bonding, it was mainly due to the hydrophobic effect of calixarene. In the mode of hydrophobic interaction, good separation of nucleosides, polycyclic aromatic hydrocarbons, monosubstituted benzene, etc. is achieved; but from the perspective of hydrophilic interaction, it is found that it has weak hydrophilicity, and the separation effect is extremely poor, basically Cannot meet the requirement of complete separation

Method used

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  • Chitosan derivatization calix [4] arene bonded silica gel stationary phase and preparing method and application thereof
  • Chitosan derivatization calix [4] arene bonded silica gel stationary phase and preparing method and application thereof
  • Chitosan derivatization calix [4] arene bonded silica gel stationary phase and preparing method and application thereof

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Embodiment Construction

[0032] Such as figure 1 所示,本发明所述的壳聚糖衍生化杯[4]芳烃键合硅胶固定相的结构式为:

[0033] .

[0034] One, chitosan derivatization calix [4] arene bonded silica gel stationary phase of the present invention can be passed such as figure 2 The preparation shown gives:

[0035] 该固定相的合成过程大致可分为三个过程:第一部分即离子液体键连壳聚糖的合成:由壳聚糖(20kDa)与3-(4-溴丁基)-1-甲基咪唑溴化物通过取代反应得到3-(4-溴丁基)-1-甲基咪唑溴化物键联壳聚糖(Ⅰ);第二部分主要是5,11,17,23-四叔丁基-25,27-二(3-溴丙氧基)-26,28-二羟基杯[4]芳烃(Ⅱ)的制备:先通过对叔丁基苯酚与甲醛在碱性条件下缩聚反应制得对叔丁基杯[4]芳烃,之后对叔丁基杯[4]芳烃与1,3-二溴丙烷通过取代反应得到5,11,17,23-四叔丁基-25,27-二(3-溴丙氧基)-26,28-二羟基杯[4]芳烃(Ⅱ);第三部分注意是通过戊二醛对硅胶表面进行改性后与3-(4-溴丁基)-1-甲基咪唑溴化物键联壳聚糖进行缩合反应,之后采用硼氢化钠还原,得到的产物再与5,11,17,23-四叔丁基-25,27-二(3-溴丙氧基)-26,28-二羟基杯[4]芳烃(Ⅱ)反应,即得到预期固定相(3-(4-溴丁基)-1-甲基咪唑溴化物键连壳聚糖衍生化杯[4]芳烃键合硅胶固定相)成品。

[0036] Two, the specific preparation method of chitosan derivatization calix[4]arene bonded silica gel stationary phase of the present invention is:

[0037] 1 ) Preparation of ionic liquid bonded chitosan (I): 在氮气气氛下制备3-(4-溴丁基)-1-甲基咪唑溴化物键联壳聚糖。将1.0g(6.21mmol)壳聚糖(20...

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Abstract

The invention discloses a chitosan derivatization calix [4] arene bonded silica gel stationary phase. Firstly, chitosan reacts with 3-(4-brombutyl)-1-methylimidazole bromide to generate 3-(4-brombutyl)-1-methylimidazole bromide bonded chitosan; p-tert-butyl calix [4] arene is obtained through condensation polymerization of p-tert-butylphenol and formaldehyde, and 5,11,17,23-tetra-tert-butyl-25,27-di(3-bromopropoxy)-26,28-dyhydroxyl calix [4] arene is obtained through substitution reaction of p-tert-butyl calix [4] arene and 1,3-dibromopropane; the surface of silica gel is modified by means of glutaraldehyde, then condensation polymerization is conducted between silica gel and 3-(4-brombutyl)-1-methylimidazole bromide bonded chitosan, then reduction is conducted by means of sodium borohydride, and the product reacts with 5,11,17,23-tetra-tert-butyl-25,27-di(3-bromopropoxy)-26,28-dyhydroxyl calix [4] arene to generate the expected stationary phase. The stationary phase is easy to prepare, wide in application range, high in reproducibility and broad is application prospects.

Description

technical field [0001] The invention relates to the technical field of functional material synthesis, in particular to a chitosan derivatized calix[4]arene bonded silica gel stationary phase, and also relates to a preparation method and application of the stationary phase. Background technique [0002] High performance liquid chromatography (HPLC) was developed rapidly after the introduction of gas chromatography theory in the late 1960s on the basis of classical liquid chromatography. Reverse-phase liquid chromatography (RPLC) is the most widely used chromatographic separation technique so far. It can be combined with various conventional detection methods to solve a variety of analytical application problems, but for some analytes, especially polar and hydrophilic Sexual compounds are little or no retained. For a long time, normal phase liquid chromatography (NPLC) has been used to analyze these substances using environmentally unfriendly non-water-soluble mobile phases s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C08B37/08B01J20/286B01J20/30
CPCB01J20/286C08B37/003C08G83/001
Inventor 张文芬张岩皓蒋琼吴宁鹏杜慧芳班付国张书胜
Owner 江苏国技仪器有限公司
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