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Preparation method for multi-mode-combined vancomycin stationary phase of chromatography

A technology of chromatographic stationary phase and vancomycin, which is applied in the field of preparation of multi-mode combined vancomycin chromatographic stationary phase, can solve problems such as obvious steric hindrance effect, achieve enhanced separation ability, improve bonding efficiency, and reduce macromolecular sites. The effect of resistance

Inactive Publication Date: 2018-05-18
南京赢点色谱分离技术有限公司
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Problems solved by technology

The advantage of this method is that the synthesis steps are simple, the operation steps are few, and the cost is relatively low. However, due to the large molecule of the macrocyclic antibiotic, the steric hindrance effect is obvious during the bonding process, and there will be a large amount of silanol residues on the surface of the silicon sphere, which will Serious negative impact on the chromatographic separation process (such as chromatographic peak tailing, broadening, etc.)

Method used

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  • Preparation method for multi-mode-combined vancomycin stationary phase of chromatography
  • Preparation method for multi-mode-combined vancomycin stationary phase of chromatography
  • Preparation method for multi-mode-combined vancomycin stationary phase of chromatography

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Embodiment 1

[0042] According to attached figure 2 In the method shown, glutaraldehyde is used as a spacer on the surface of silica gel, and vancomycin is bonded to prepare a multi-mode chiral chromatography stationary phase. The specific preparation steps are:

[0043] (1) Pretreatment of silica gel microspheres

[0044] Get 20g of silica gel microspheres (particle diameter 5μm, pore diameter ), dispersed in 0.1mol / L sodium hydroxide solution, after ultrasonication for 30min, add dilute hydrochloric acid to adjust the pH value to 6.5-7, wash thoroughly with water, wash three times with methanol or acetonitrile, dry at 50°C, and set aside .

[0045] (2) Silanization treatment of silica gel microspheres

[0046] Disperse the silica gel particles activated in step (1) in 80mL of methanol-water (volume ratio: 7:1) solution, add 20mL of APTES reagent in turn, after ultrasonic mixing, reflux at 65°C for 24h, wash with methanol for 3 times , and dried to obtain amino-modified silica sphere...

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Abstract

The invention relates to a preparation method for a multi-mode-combined vancomycin stationary phase of chromatography. The preparation method comprises the following steps: modifying the surface of asilicon sphere with an amino group; then with glutaraldehyde as a spacer, bonding the macrocyclic glycopeptide antibiotic vancomycin onto the surface of the silicon sphere through an aldimine condensation reaction; and carrying out bonding and terminating by using small-molecular amino acids or sugar so as to prepare the multi-mode-combined chiral stationary phase of chromatography. A vancomycin structure has a plurality of function groups and is applicable to separation operation in different chromatographic separation modes; moreover, glutaraldehyde is used as the spacer for bonding the macrocyclic glycopeptide antibiotic onto the surface of the silicon sphere, so steric-hinerance effect is effectively reduced and bonding efficiency is improved; and termination via small molecules can shield the negative effect of residual silicon hydroxyl groups in chromatographic separation, provide more action sites of different types and improve separation efficiency and separation selectivity.

Description

technical field [0001] The invention relates to the technical field of textile production, in particular to a method for preparing a multi-mode combined vancomycin chromatographic stationary phase. Background technique [0002] Vancomycin, as a macrocyclic antiglycopeptide antibiotic, has a variety of functional groups. Its structure contains 3 cavities, 18 chiral centers, carboxyl groups, amide groups, glycoside groups, etc. Studies have shown that, The vancomycin-bonded modified stationary phase is suitable for chiral resolution in various chromatographic separation modes such as reversed phase, normal phase, hydrophilic, polar-organic, etc. [0003] Due to its complex and diverse mechanism of action, vancomycin bonded stationary phase can realize the separation of complex systems such as biological samples, and has a very wide application potential. It can be applied to the chromatographic separation of components such as proteins and peptides, and can also be used in tra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/29B01J20/30B01D15/38
CPCB01D15/3833B01J20/29
Inventor 张维冰张麟刘翻
Owner 南京赢点色谱分离技术有限公司
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