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Preparation of polynary cyclodextrin polymer and application thereof to CE chiral analysis

A technology of cyclodextrin polymer and cyclodextrin, which is applied in the direction of material analysis, analysis materials, instruments, etc. by electromagnetic means, can solve the problems of limited wide application and low water solubility, and save time and energy, reduce cost effect

Inactive Publication Date: 2017-06-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The most commonly used cyclodextrin is β-cyclodextrin, but its low water solubility limits its wide application

Method used

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  • Preparation of polynary cyclodextrin polymer and application thereof to CE chiral analysis
  • Preparation of polynary cyclodextrin polymer and application thereof to CE chiral analysis
  • Preparation of polynary cyclodextrin polymer and application thereof to CE chiral analysis

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preparation example Construction

[0047] (3) Preparation of CM-α, β, γ-CDP: Add 12.6g sodium hydroxide to 42mL water, stir to dissolve and cool down to room temperature, add 6g CM-α-CD, 7g CM-β-CD and 8g carboxymethyl - γ-cyclodextrin polymer powder, stirred at room temperature for 0.5h, added 18.9mLECH, heated to 75°C, and reacted for 3h. After the reaction solution was cooled to room temperature, the pH was adjusted to neutral with dilute hydrochloric acid, poured into a dialysis bag with a molecular weight cut off of 7000 for dialysis for 2 days, and dried by rotary evaporation to obtain the final product CM-α,β,γ-CDP polymer.

[0048] The characterization of polycyclodextrin polymer comprises the following steps:

[0049] (1) Preparation of color developer: Weigh 100 mg of blue tetrazolium into a beaker, add 50 mL of 0.1 mol / L sodium hydroxide solution, dissolve by ultrasonication for 30 s, and heat in a 60°C water bath with stirring until the solution is yellow and transparent. After cooling down slightl...

Embodiment 1

[0060] The application of SPE-α, β, γ-CDP in CE chiral separation includes the following steps:

[0061] Use Tris (Tris) and phosphoric acid to prepare reference buffers with different pH, filter through a 0.45 μm filter membrane, and set aside. A certain amount of SPE-α, β, γ-CDP was weighed and added to the buffer solution to prepare a running buffer solution with a mass volume concentration ratio of 2% for later use. After the capillary was activated, warfarin, ofloxacin, amlodipine and promethazine were separated using SPE-α, β, γ-CDP as the resolving agent. Separation conditions: uncoated capillary, effective length / total length 30cm / 37cm, inner diameter 50μm, detection wavelength 214nm, temperature 37℃, buffer pH 2.5, 20mmol / L Tris-H 3 PO 4 buffer solution, the separation voltage is -11kV, and the mass-volume concentration ratio of the chiral resolving agent is 2%. (Such as Picture 1-1 , Figure 1-2 , Figure 1-3 and Figure 1-4 ).

Embodiment 2

[0063] The application of CM-α, β, γ-CDP in CE chiral separation includes the following steps:

[0064] Use Tris and phosphoric acid to prepare reference buffer solutions with different pHs, filter them through a 0.45 μm filter membrane, and set aside. A certain amount of CM-α, β, γ-CDP was weighed and added to the buffer solution to prepare a running buffer solution with a mass volume concentration ratio of 2% for later use. After the capillary was activated, warfarin, verapamil, propranolol and ofloxacin were separated using CM-α, β, γ-CDP as the resolving agent. Separation conditions: uncoated capillary, effective length / total length 30cm / 37cm, inner diameter 50μm, detection wavelength 214nm, temperature 37℃, buffer pH 2.5, 20mmol / L Tris-H 3 PO 4 buffer solution, the separation voltage is +11kV, and the mass volume concentration ratio of the chiral resolving agent is 2% ( diagram 2-1 , Figure 2-2 , Figure 2-3 and Figure 2-4 )

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Abstract

The invention discloses a preparation method of a polynary cyclodextrin polymer. Different derivatization cyclodextrins are polymerized to prepare binary gamma-cyclodextrin polymer sulfopropyl ether-gamma-cyclodextrin polymers, carboxymethyl-gamma-cyclodextrin polymers and sulfopropyl ether-alpha, beta, gamma-cyclodextrin polymers or carboxymethyl-alpha, beta, gamma-cyclodextrin polymers. The cyclodextrin polymer are used as chiral resolving agents to be added into an electrophoretic buffer solution for separating chiral medicine so as to obtain the wide separation application. The polynary cyclodextrin polymer chiral resolving agents can be recovered and reutilized by a dialysis method. Through the optimization on the separation conditions, including the cyclodextrin polymer concentrate, buffer solution pH, separation voltage, organic additives and the like, the randomly selected chiral medicine reaches the base line separation. The preparation method is favorable for determining the separation and analysis method of unknown compounds in the future industrial production through simple trail; the time and the energy are saved for the practical production; the cost is reduced.

Description

technical field [0001] The invention relates to the synthesis of binary or multi-component cyclodextrin polymer chiral resolving agent and its application in capillary electrophoresis chiral analysis. Background technique [0002] Compared with high performance liquid chromatography and gas chromatography, capillary electrophoresis (CE) has the advantages of high efficiency, rapidity, small sample volume, high selectivity, various separation modes and easy automation, and is widely used in the field of chiral separation. . [0003] For CE chiral separation, the use of chiral resolving agents to construct a stereoselective environment is the key to achieve enantiomeric distinction. There are many kinds of chiral resolving agents, among which cyclodextrin and its derivatives are the most widely used class of chiral resolving agents. Natural cyclodextrin and its neutral derivatives have successfully separated some chiral compounds, but their low solubility and difficulty in s...

Claims

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Application Information

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IPC IPC(8): C08B37/16C08G59/04G01N27/447
CPCC08B37/0012C08G59/04G01N27/447
Inventor 李优鑫包建民贾菲菲李雪
Owner TIANJIN UNIV
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