Alanine substituted calix[4]arene bonded silica stationary phase and preparation method and application thereof

A technology for bonding silica gel and alanine, which is applied in the field of separation science, can solve the problems of limited performance of bonded phases and few types of calixarene bonded phases, and achieves good identification and separation performance, high bonding amount and stable performance. Effect

Inactive Publication Date: 2012-06-13
ZHENGZHOU UNIV
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Problems solved by technology

[0007] However, due to the fact that there are few types of calixarene bonded phases, the performance of bonded phases is limited, and there are many substanc

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  • Alanine substituted calix[4]arene bonded silica stationary phase and preparation method and application thereof
  • Alanine substituted calix[4]arene bonded silica stationary phase and preparation method and application thereof
  • Alanine substituted calix[4]arene bonded silica stationary phase and preparation method and application thereof

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preparation example Construction

[0031] 2. Preparation of γ-aminopropyltrimethoxy bonded silica gel

[0032] Take 5.0 mL of γ-aminopropyltrimethoxysilane in a 500 mL three-neck round bottom flask, add 200 mL of freshly distilled anhydrous toluene, add 10.0 g of activated silica gel under magnetic stirring, and add 0.4 mL of triethylamine (anhydrous ), install the return line and CaCl 2 Dry the tube and reflux for 24 h under nitrogen protection. Stop the reaction, filter with a G5 sand core funnel, wash with toluene, acetone, double-distilled water, and acetone in sequence, and dry in vacuum at 80°C for 8 h to obtain γ-aminopropyltrimethoxy bonded silica gel.

[0033] 3. Preparation of 25,27-bis(L-alanine methyl ester-N-carbonylmethoxy)-26,28-dihydroxy-p-tert-butylcalix[4]arene bonded stationary phase

[0034]Weigh 3.0 g of 25,27-bis(L-alanine methyl ester-N-carbonylmethoxy)-26,28-dihydroxy-p-tert-butylcalix[4]arene in a 100 mL three-neck round bottom flask , add 50 mL freshly steamed anhydrous toluene, und...

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Abstract

The invention relates to an alanine substituted calix[4]arene bonded silica stationary phase and a preparation method and application thereof. According to the invention, gamma-aminopropyl trimethoxy silane is used as a coupling agent and reacts with specially-produced silica gel under the protection of triethylamine and inert gas so as to prepare gamma-aminopropyl trimethoxy bonded silica which reacts with 25,27-di(L-alanine methyl ester-N-carbonyl-methoxy)-26,28-dihydroxy-p-tert-bytyl-calix[4]arene under the protection of triethylamine and inert gas so as to prepare the alanine substituted calix[4]arene bonded silica stationary phase. The alanine substituted calix[4]arene bonded silica stationary phase prepared in the invention has the advantages of high bonded amount, stable performance and better separation selectivity, has same performance as traditional ODS reversed phase chromatography does, provides a plurality of action sites for inclusion, complexation, hydrogen bonding, etc. and is advantageous in separation of specific substances difficult to separate.

Description

technical field [0001] The invention relates to an alanine-substituted calix[4]arene bonded silica gel stationary phase and a preparation method and use thereof, which belong to functional material synthesis technology and are suitable for separation science and technology fields such as high-performance liquid chromatography. Background technique [0002] With the development of separation science, high performance liquid chromatography is widely used in petroleum, chemical industry, environmental protection, food, medicine, legal inspection, clinical and natural product analysis due to its high sensitivity, high selectivity, high column efficiency, good repeatability and easy operation. Among them, it plays a very important role and becomes an important technique for separating complex samples. In recent years, with the rapid development of science and technology, the separation system studied has become more and more complex, especially the separation of positional isomer...

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Application Information

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IPC IPC(8): B01J20/286B01J20/30
Inventor 张书胜刘军伟胡锴赵文杰王磊李海斌吴养洁
Owner ZHENGZHOU UNIV
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