Overall chiral stationary phase of silica gel capillary and preparation method thereof

A technology of chiral stationary phase and capillary monolithic column, which is applied in chemical instruments and methods, and other chemical processes, and can solve the problems of large consumption, chiral reagents that cannot be reused, and chiral immobilization of rosin-based derivatives. , to achieve the effect of low cost, wide solvent selectivity and easy operation

Inactive Publication Date: 2010-07-07
GUANGXI NORMAL UNIV
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  • Description
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Problems solved by technology

However, in the chiral separation mode of capillary electrophoresis, chiral reagents cannot be reused, and the consumption is large, and a charged chiral selector i

Method used

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  • Overall chiral stationary phase of silica gel capillary and preparation method thereof
  • Overall chiral stationary phase of silica gel capillary and preparation method thereof
  • Overall chiral stationary phase of silica gel capillary and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment

[0024] (1) Synthesis of maleopimaric acid:

[0025] Take 30.2g of ground-grade rosin in a large beaker, heat it up to 140°C, slowly add 8.82g of maleic anhydride and 1.92g of p-toluenesulfonic acid under constant stirring, then raise the temperature to 180°C, keep it warm for 3 hours, and Pour out heat, grind after cooling, then recrystallize 3 times with glacial acetic acid, filter, and dry to obtain maleopimaric acid (yield 52%), m.p.228-230°C;

[0026] (2) Preparation of silica gel capillary monolithic column:

[0027] Take a quartz capillary with an inner diameter of 75 μm and an outer diameter of 365 μm, soak it with 1mol / L NaoH solution overnight, rinse with secondary water, hydrochloric acid, secondary water, acetone, and anhydrous ether for 1 hour, and then dry it at 180°C for 3 hours under nitrogen flow , sealed at both ends for subsequent use, 0.22g of polyethylene glycol (Mr=10000), 0.225g of urea were dissolved in 0.01mol / L acetic acid solution, wherein 1mL of tet...

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Abstract

The invention discloses an overall chiral stationary phase of silica gel capillary and a preparation method thereof. The preparation method is characterized by comprising the following steps: preparing a novel chiral group maleopimaric acid through reaction of natural chiral rosin and maleic anhydride, and synthesizing the novel chiral group maleopimaric acid onto a carrier through chemical bonds with propyl amine as a connecting unit of the novel chiral group and an overall column carrier of a silica gel-based capillary. The invention is applicable to the stationary phase of electrochromatography or liquid-phase chromatography of the capillary. Moreover, the invention has the advantages that: the cost of the prepared chiral stationary phase is low, the column efficiency is high, the scope of application is wide for various mobile phases, the manufacture is simple and rapid, and the commercial production can be realized.

Description

technical field [0001] The invention relates to the preparation of a chromatographic stationary phase, in particular to a preparation method of a novel silica gel capillary chiral monolithic stationary phase. Background technique [0002] The enantiomer of chiral substances plays an important role in the process of human life. Many substances closely related to human life, such as proteins, polypeptides, amino acids and chiral drugs, have one or more chiral centers. Different enantiomers have different optical activities and three-dimensional conformations, and exhibit different physiological and pharmacological activities in vivo. Therefore, the chiral separation of enantiomers is of great significance in life science and other related fields. There are many preparation methods for chiral stationary phases, some of which are not widely used, some have poor solvent selectivity, and some have many reaction steps, are complicated and difficult to operate. At present, capilla...

Claims

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Application Information

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IPC IPC(8): B01J20/285B01J20/30
Inventor 叶芳贵王恒山赵书林黄保军
Owner GUANGXI NORMAL UNIV
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