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Tween type hydrophilic interaction chromatographic stationary phase as well as synthesis and application thereof

A chromatographic stationary phase and a technique for hydrophilic interaction, which is applied in the design field of Tween-like hydrophilic interaction chromatography stationary phases, and can solve problems such as insufficient hydrophilicity and unfavorable application.

Inactive Publication Date: 2015-06-10
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the complexity of actual samples and the diversity of separation requirements, there is no hydrophilic interaction chromatography that can meet the separation requirements of most polar compounds. Therefore, it is very important to develop a new hydrophilic interaction chromatography stationary phase. Work
Polyethylene glycol column (PEG column) is a commercialized hydrophilic interaction chromatographic column. This chromatographic column mainly uses the hydrophilicity of polyethylene glycol groups to achieve chromatographic separation, but its hydrophilicity Insufficient shortcomings, and the hydrophobic effect accumulated by the fatty chain is too strong, so that it shows the characteristics of the mixed mode of hydrophilic interaction chromatography and reversed-phase chromatography, which is not conducive to its application in the hydrophilic interaction chromatography mode [Document 6: P .Jander, T.Hájek, J.Sep.Sci.32(2009)3603. Document 7: E.Blahová, P.Jandera, F.Cacciola, L.Mondello, J.Sep.Sci.29(2006)555. ]

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  • Tween type hydrophilic interaction chromatographic stationary phase as well as synthesis and application thereof
  • Tween type hydrophilic interaction chromatographic stationary phase as well as synthesis and application thereof
  • Tween type hydrophilic interaction chromatographic stationary phase as well as synthesis and application thereof

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Embodiment Construction

[0022] The present invention also relates to the preparation method of above-mentioned chromatographic stationary phase, and synthetic route is as follows:

[0023]

[0024] The specific operation steps are as follows:

[0025] (1) Dissolve 20ml of Tween (Tween20, 40, 60 or 80) in 100ml of anhydrous toluene, and add 4.0g of silane reagent (EtO) dropwise to the above solution through the dropping funnel at 80°C 3 SiCH 2 CH 2 CH 2 NCO, continue to react for 8h after the dropwise addition is completed;

[0026] (2) Add 6.0g of dry silica gel and 1ml of anhydrous pyridine to the solution obtained from the reaction in (1), and reflux for 24h;

[0027] (3) After cooling, filter, and wash the solid product successively with a large amount of toluene, ethanol, water, ethanol and acetone, and then vacuum-dry at 60°C for 8 hours to obtain the target stationary phase.

[0028] The elemental analysis results are shown in Table 1. The results show that Tween is successfully bonded ...

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Abstract

The invention relates to synthesis of a Tween type hydrophilic interaction chromatographic stationary phase and application of the Tween type hydrophilic interaction chromatographic stationary phase to a hydrophilic interaction chromatography. Tween is used as an initiator and the target hydrophilic interaction chromatographic stationary phase is conveniently and rapidly synthesized by two-step reaction. The novel hydrophilic interaction chromatographic stationary phase is correspondingly applied to the hydrophilic interaction chromatography, and has a good separation property in separated polar compounds and water-soluble compounds.

Description

technical field [0001] The invention relates to the design of Tween-like hydrophilic interaction chromatographic stationary phase. [0002] The present invention also relates to a preparation method of the above-mentioned stationary phase. [0003] The present invention also relates to the application of the above stationary phase in hydrophilic interaction chromatography. Background technique [0004] In the traditional liquid chromatography separation mode, reversed-phase chromatography using C8 / C18 stationary phase is the most commonly used, it can meet the needs of most chromatographic separations, but reversed-phase chromatography is difficult to separate highly polar compounds, because such polarity Compounds are extremely weakly retained on C8 / C18 stationary phases and tend to elute at dead times. In order to solve the problem of liquid phase separation of such strong polar compounds, hydrophilic interaction chromatography came into being [Document 1: D.García-Gómez...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01J20/30B01D15/08
Inventor 肖红斌用天万伯顺
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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