Self-assembled cyclodextrin functionalized magnetic-gold composite material as well as preparation method and application thereof

A composite material and cyclodextrin technology, which is applied in the field of functional materials and chiral separation, can solve the problems of difficult control of bonding reaction and low bonding rate, and achieve controllable preparation methods, rapid separation and regeneration, and high-efficiency separation Effect

Inactive Publication Date: 2020-06-05
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the bonding reaction is not easy to control, the bonding rate is generally low, which limits its practical application.

Method used

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  • Self-assembled cyclodextrin functionalized magnetic-gold composite material as well as preparation method and application thereof
  • Self-assembled cyclodextrin functionalized magnetic-gold composite material as well as preparation method and application thereof
  • Self-assembled cyclodextrin functionalized magnetic-gold composite material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1—Preparation method of self-assembled cyclodextrin functionalized magnetic-gold composite microspheres

[0039] (1) Magnetic Fe 3 o 4 Preparation of @PN submicrospheres

[0040] Weigh 1.35g of FeCl 3 ·6H 2 Dissolve O in 40 mL of ethylene glycol, add 3.6 g of anhydrous sodium acetate and 1 g of polyethylene glycol-6000 in sequence, and stir magnetically for 0.5 h. The resulting solution was transferred to a 50 mL stainless steel reaction kettle, and heated to 200° C. for 8 h. The product was collected with the assistance of an external magnetic field, washed with deionized water and ethanol three times, 50 mL each time, to obtain a magnetic Fe 3 o 4 submicrospheres. The prepared magnetic Fe 3 o 4 1.0 g of magnetic microspheres was redispersed into 500 mL of aqueous solution, and then 2 g of tris, 1.2 g of norepinephrine were added, the mixture was ultrasonicated in a water bath for 10 min, and mechanically stirred for 8 h at room temperature at 25 ° C t...

Embodiment 2

[0048] Embodiment 2—Structural characterization of magnetic materials

[0049] (1) Particle morphology, particle size and characterization

[0050]The particle size and morphology of the prepared magnetic particles were observed with a Tecnai G2F20 transmission electron microscope (FEI, USA). figure 1 A transmission electron microscope (TEM) image of a magnetic material and gold nanoparticles. It can be seen from the figure that the Au nanoparticles are spherical with an average particle size of 3nm. Magnetic Fe 3 o 4 The @PN / Au / β-CD composite material is spherical, with an average particle size of 300±10nm, and the outer layer is wrapped with a layer of polynorepinephrine with a thickness of 20±5nm. The Au nanoparticles are evenly distributed in the Fe 3 o 4 / PN surface.

[0051] (2) Element characterization

[0052] The X-ray energy loss spectrum of the magnetic microspheres was measured by an X-ray energy spectrometer (TEM accessory, FEI Company, USA). figure 2 is ...

Embodiment 3

[0059] Example 3 Self-assembled magnetic Fe 3 o 4 Separation of mandelic acid from @PN / Au / β-CD composites

[0060] The self-assembled magnetic Fe prepared by the technical scheme of the present invention 3 o 4 The @PN / Au / β-CD composite is a chiral adsorbent for the separation of mandelic acid enantiomers in aqueous solution.

[0061] RS-mandelic acid was selected as the analyte, and the separation effect was analyzed by HPLC. Use n-hexane-isopropanol (8:2) to prepare a standard solution with a mass concentration of mandelic acid of 1 μg / L, and take 20 μL of this solution for liquid chromatography (the instrument model is Shimazu HPLC-20A, and the manufacturer is Shimadzu Corporation, Japan. The instrument is equipped with SPD-M20A diode array detector, CTO-20AC column thermostat, SIL-20AC autosampler; the chromatographic column is Chiralcel OD-H chiral column (250mm×4.6mm I.D, 5.0μm particles). The business is Daicel Pharmaceutical Chiral Technology (Shanghai) Co., Ltd.; ...

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Abstract

The invention discloses a self-assembled cyclodextrin functionalized magnetic-gold composite material as well as a preparation method and application thereof. The preparation method comprises the following steps: preparing diamino-modified magnetic Fe3O4@SiO2 sub-microspheres by utilizing solvothermal reduction, TEOS hydrolysis and silanization reaction; preparing gold nanoparticles by adopting asodium borohydride reduction chloroauric acid method, mixing the gold nanoparticles with the diamino-modified magnetic Fe3O4c sub-microspheres to obtain a more stable magnetic gold nanoparticle compound by utilizing coordination and chelation of diamino on the surfaces of the magnetic sub-microspheres and the gold nanoparticles. Meanwhile, sulfhydrylated beta-cyclodextrin is prepared and is fixedon the surface of the magnetic Fe3O4@SiO2 / Au composite material through an Au-S bond, so that the magnetic functional composite material is prepared. A magnetic nano material is used as a chiral selector carrier and combined with a self-assembly technology as a fixing mode to prepare a chiral recognition material, so that the defects of stability and loading capacity of a chiral stationary phase are expected to be improved, and rapid screening of a chiral selector and efficient and high-capacity chiral separation are realized.

Description

technical field [0001] The invention belongs to the technical field of functional materials and chiral separation, and more specifically relates to a self-assembled cyclodextrin functionalized magnetic-gold composite material and its preparation method and application in chiral separation. Background technique [0002] The two enantiomers of chiral compounds have the same physical and chemical properties except optical activity, but their biochemical and pharmacological activities are often different, or even have opposite effects. Therefore, the study of chiral separation technology is of great significance to the pharmaceutical industry and life science. Chiral resolution technology mainly includes mechanical resolution, preferential crystallization, chemical resolution, enzymatic resolution, membrane separation and chromatographic resolution and other resolution methods. Among them, the liquid chromatography chiral stationary phase resolution method is considered to be t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16C08G83/00C07C59/50C07C51/47B01J20/26B01J20/28B01J20/32B01D15/38
CPCB01D15/3833B01J20/0233B01J20/06B01J20/24B01J20/262B01J20/28009B01J20/3204B01J20/3231C07B2200/07C07C51/47C08B37/0012C08G83/001C07C59/50
Inventor 邓小娟陈小平李文斌
Owner TIANJIN UNIV
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