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Phosphate radical containing cotton modification material and preparation method and application thereof

A technology of modifying materials and phosphate radicals, which is applied in the field of analytical chemistry, can solve the problems of low modification amount of functional groups and the influence of adsorbent adsorption capacity, etc., and achieve the effects of less solvent consumption, increased practicability, and simple operation

Active Publication Date: 2017-05-10
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the previous modification methods generally have the problem of low modification amount of functional groups, which will have a certain impact on the adsorption capacity of the adsorbent.

Method used

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  • Phosphate radical containing cotton modification material and preparation method and application thereof
  • Phosphate radical containing cotton modification material and preparation method and application thereof
  • Phosphate radical containing cotton modification material and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] [Example 1] CF-NH 2 - Preparation of AZO-p(VPA-x)

[0037] First prepare amino-modified cotton to obtain CF-NH2 ; Then connect the free radical initiator to CF-NH 2 On, get CF-NH 2 -AZO; then surface-initiated polymerization in CF-NH 2 -AZO surface modified phosphate to get CF-NH 2 -AZO-p(VPA-x), as attached figure 1 shown.

[0038] where CF-NH 2 The preparation method is as follows: Weigh 0.5g of ethylenediaminetetraacetic dianhydride (EDTAD) into a 500mL round bottom flask, add 300mL of anhydrous N’N-dimethylamide (DMF), and then add 1.0g of absorbent cotton. After thorough mixing, react at 130° C. for 6 h under the condition of magnetic stirring. After the reaction was completed, it was cooled for a period of time, and the reaction liquid was poured out, and 300 mL of DMF was added again, and then 0.5 mL of ethylenediamine was added, and the reaction was carried out at 70° C. for 4 h under magnetic stirring conditions. The product was washed successively with...

Embodiment 2

[0041] [Example 2] CF-NH 2 -AZO-p(VPA-x)-M n+ preparation of

[0042] Prepare titanium sulfate aqueous solution (0.1M), zirconium oxychloride aqueous solution (0.1M), ferric chloride aqueous solution (0.1M) each 20mL, add 0.2g CF-NH to these three solutions respectively 2 -AZO-p(VPA-2), shake at room temperature for 5 hours. The product was washed successively with ethanol, water and acetone, and dried under vacuum at 60°C.

Embodiment 3

[0043] [Example 3] Three kinds of CF-NH 2 -AZO-p(VPA-2)-M n+ (M n+ = Ti 4+ , Zr 4+ ,Fe 3+ ) were applied to the selective enrichment of phosphorylated peptides in β-casein hydrolyzate

[0044] β-casein was prepared into a 1 mg / mL solution with 100 mM Tris-HCl (pH 8.5). Add trypsin to the above solution according to the ratio of enzyme to substrate ratio of 1:50 (w / w), and react at 37°C for 16h. The polypeptide product after enzymatic hydrolysis was drained by a vacuum centrifugal concentrator and stored in a -20°C refrigerator for later use.

[0045] Accurately weigh 5mg CF-NH2-AZO-p(VPA-2)-M n+ Extractions were performed in 1-mL disposable syringe needles. Use already balanced CF-NH 2 -AZO-p(VPA-2)-M n+ Repeatedly extract 100 μL of the mixture containing the peptide (3% TFA-50% ACN (v / v)). After washing twice with the sample solution, the analytes on the material were desorbed with 100 μL desorption solution (2.5% NH 3 ·H 2 O) Desorb into a centrifuge tube. Afte...

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Abstract

The invention belongs to the field of analytical chemistry. A novel phosphate radical containing cotton modification material is prepared by adopting a graft copolymerization method. The phosphorus content of the material can be well controlled by adjusting the content of a monomer VPA, then metal ions are immobilized on the material, and the material can serve as a material for fixing metal affinity chromatography and used for selective enrichment of phosphorylated polypeptides in multiple biological samples. The optimal material CF-NH2-AZO-p(VPA-2)-Ti4+ can be optimized by researching the relation between the content of phosphate radical groups in the material and material extracting capability. The material has the high selectivity and high extraction capability to the phosphorylated polypeptides in a standard polypeptide mixed solution, milk enzymatic hydrolysate, serum and rat brain lysate. Therefore, application of the graft copolymerization method in cellulose post-modification can be promoted, and application of a cellulose adsorbent in bioanalysis is widened.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a cotton modification material containing phosphate radicals and the application of the material as a solid-phase extraction adsorbent after being loaded with metal ions. Background technique [0002] Cellulose is a linear polymer composed of β-D-glucose units, containing a large number of hydroxyl groups (three hydroxyl groups per glucose unit). As the most abundant natural polymer material, cellulose is environmentally friendly, inexpensive, biocompatible, and highly porous. Cellulose is widely used in many fields, such as catalyst material, filter membrane material and adsorbent material. As a cellulose material, cotton has more advantages than cellulose, and has received great attention in recent years. [0003] In our previous work, a variety of cotton-related functionalized materials were developed and used for the selective enrichment of target analytes in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M13/342D06M13/332D06M15/356C07K1/14B01J20/285B01J20/30D06M101/06
CPCB01J20/285B01J20/30C07K1/145D06M13/332D06M13/342D06M15/3564D06M2101/06
Inventor 冯钰锜何小梅
Owner WUHAN UNIV
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