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Preparation method and application of chiral bonded capillary electrochromatography open tubular column

A technology of capillary electrochromatography and open-tube columns, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of easy detachment of stationary phase and short service life, so as to improve mechanical strength and stability, increase sample capacity, increase Effect of Column Efficiency and Separation Selectivity

Active Publication Date: 2018-06-19
QIQIHAR UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the open-tubular column prepared by coating, the stationary phase is easy to fall off and has a short service life; while in the open-tubular column prepared by bonding, the stationary phase is firmly bonded to the inner wall of the capillary through chemical bonds, which can overcome this problem. Weaknesses and deficiencies

Method used

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  • Preparation method and application of chiral bonded capillary electrochromatography open tubular column
  • Preparation method and application of chiral bonded capillary electrochromatography open tubular column
  • Preparation method and application of chiral bonded capillary electrochromatography open tubular column

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preparation example Construction

[0029] The invention provides a preparation method of a chiral bonded capillary electrochromatographic open column, the process flow is as follows figure 1 As shown, the specific steps are:

[0030] (1) Preparation of single-6-p-toluenesulfonyl β-cyclodextrin:

[0031] Dissolve 5.0g of β-cyclodextrin (β-CD) in 100mL of 30% sodium hydroxide solution, add 1.5-1.8g of p-toluenesulfonyl chloride in a cold water bath, stir for 4-6 hours, filter, and use 1mol / L HCl solution adjusted the pH of the filtrate to 6-7, and a white precipitate precipitated out. The mixture was placed in a refrigerator (0-4°C) overnight, filtered, and the precipitate was recrystallized twice with distilled water, acetonitrile:water (volume ratio 1:1) Recrystallize once and dry under vacuum at 50°C to obtain mono-6-p-toluenesulfonyl β-cyclodextrin (6-OTs-β-CD).

[0032] (2) Preparation of mono-6-ethylenediamino-β-cyclodextrin

[0033] Weigh 3.0g 6-OTs-β-CD, add 40~50mL ethylenediamine, stir to dissolve, r...

Embodiment 1

[0047] In this embodiment, the preparation method of chiral bonded capillary electrochromatography open-tubular column, the specific steps are as follows:

[0048] (1) Preparation of single-6-p-toluenesulfonyl β-cyclodextrin:

[0049] Dissolve 5.0g of β-CD in 100mL of 30% sodium hydroxide solution, add 1.6g of p-toluenesulfonyl chloride in a cold water bath, stir for 5 hours, filter, and adjust the pH of the filtrate to 6-7 with 1mol / L HCl solution. Precipitation was precipitated, the mixture was placed in a refrigerator (0-4°C) overnight, filtered, the precipitate was recrystallized twice with distilled water, acetonitrile:water (volume ratio 1:1) was recrystallized once, and vacuum-dried at 50°C to obtain a single - 6-p-toluenesulfonyl β-cyclodextrin (6-OTs-β-CD).

[0050] (2) Preparation of mono-6-ethylenediamino-β-cyclodextrin

[0051] Weigh 3.0g of 6-OTs-β-CD, add 45mL of ethylenediamine, stir to dissolve, react at 80°C for 4h, add acetone to precipitate a white precipi...

Embodiment 2

[0068] In this embodiment, the preparation method of chiral bonded capillary electrochromatography open-tubular column, the specific steps are as follows:

[0069] (1) Preparation of single-6-p-toluenesulfonyl β-cyclodextrin:

[0070] Dissolve 5.0g of β-CD in 100mL of 30% sodium hydroxide solution, add 1.6g of p-toluenesulfonyl chloride in a cold water bath, stir for 6 hours, filter, adjust the pH of the filtrate to 6-7 with 1mol / L HCl solution, and have a white Precipitation was precipitated, the mixture was placed in a refrigerator (0-4°C) overnight, filtered, the precipitate was recrystallized twice with distilled water, acetonitrile:water (volume ratio 1:1) was recrystallized once, and vacuum-dried at 50°C to obtain a single - 6-p-toluenesulfonyl β-cyclodextrin (6-OTs-β-CD).

[0071] (2) Preparation of mono-6-ethylenediamino-β-cyclodextrin

[0072] Weigh 3.0g of 6-OTs-β-CD, add 45mL of ethylenediamine, stir to dissolve, react at 80°C for 4h, add acetone to precipitate a ...

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Abstract

The invention discloses a preparation method and application of chiral bonded capillary electrochromatography open tubular column, which belongs to the technical field of the preparation of capillaryelectrochromatographic columns. By utilizing a special structure and molecular characteristics of beta-cyclodextrin, a derivative with an isocyanate group is designed and bonded with the inner wall ofan amination capillary tube, and a chiral capillary electrochromatogrpahy open tubular column which meets the electrochromatography separation requirement and is simple in method and good in reproducibility and stability is prepared. A stationary phase is firmly bonded onto the inner wall of the capillary tube by virtue of a chemical bond, and compared with the coated stationary phase, the mechanical strength and the stability are better.

Description

technical field [0001] The invention belongs to the technical field of capillary electrochromatographic column preparation, in particular to a preparation method and application of a chiral bonded capillary electrochromatographic open column. Background technique [0002] Chirality exists widely in nature and is a basic feature of biological systems, but human understanding and research on chiral substances are still very shallow. In recent years, as people pay more and more attention to fields related to people's livelihood, such as medicine, food, life science and environmental analysis, a large number of chiral analysis detection problems in these fields have become increasingly prominent [Analytica ChimicaActa, 931(2016): 1 -twenty four]. [0003] Chromatography is currently the most effective method for chiral separation detection methods. Among them, capillary electrochromatography, as an efficient and fast chromatographic micro-separation technology emerging in rece...

Claims

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Application Information

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IPC IPC(8): G01N30/60G01N30/02
CPCG01N30/02G01N30/6078
Inventor 高立娣李雪秦世丽唐艺旻戴强李英杰
Owner QIQIHAR UNIVERSITY
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