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A kind of nano cuprous sulfide modified monolithic column material and preparation method thereof

A cuprous sulfide and monolithic column technology, which is applied in chemical instruments and methods, separation methods, and other chemical processes, can solve the limitations of metal oxide affinity chromatography, the inability to use target molecules for affinity enrichment, and poor stability of oxides and other problems, to achieve the effects of easy production, increased specific surface area, and strong adsorption

Active Publication Date: 2017-02-08
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the poor stability of metal oxides such as copper, they cannot be used for affinity enrichment of target molecules, which limits the development and application of metal oxide affinity chromatography.
However, the stability of most metal sulfides is good, and the adsorption properties of zinc sulfide to histidine-modified proteins have been reported (Sapsford, K.E.; Pons, T.; Medintz, I.L.; et al., J. Phys.Chem.C2007,111,11528-11538), indicating that metal sulfides may be used as affinity enrichment materials

Method used

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  • A kind of nano cuprous sulfide modified monolithic column material and preparation method thereof
  • A kind of nano cuprous sulfide modified monolithic column material and preparation method thereof
  • A kind of nano cuprous sulfide modified monolithic column material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1: Preparation of monolithic column modified by nano-cuprous sulfide

[0030] Synthesis of the hybrid monolithic column skeleton: wash the quartz capillary with an inner diameter of 530 μm with HCl (0.1mol / L) for 2 hours, wash with water until neutral, wash with 1mol / L NaOH solution for 10 hours, and then wash with water and methanol respectively 0.5 hours, dry at 160°C under nitrogen for 5 hours, then fill the capillary with methanol / 3-(trimethoxysilyl)propyl methacrylate (1:1, v / v), keep at 50°C for 20 hours, washed with methanol for 1 hour, dried at 60°C under nitrogen for 1 hour, and sealed at both ends for use.

[0031] Add 120mg of methacryloyl-POSS cage mixture, 850μL of tetrahydrofuran, 120mg of Pluronic F127, 40μL of vinylimidazole into the centrifuge tube, dissolve it completely by ultrasonication, then add 2.5mg of azobisisobutyronitrile, and pour it into the capillary after ultrasonication . Both ends were sealed with silica gel and reacted at 60°C...

Embodiment 2

[0036] Example 2: Comparison of the adsorption effect of nano-cuprous sulfide modified monolithic column with commercial copper ion column and nickel ion column in the adsorption of kanamycin sulfate

[0037] Take 0.5mL nickel ion chelation column material (Ni Sepharose6Fast Flow, GE Healthcare), wash with buffer A (20mM PBS, 0.5M sodium chloride, 50mM EDTA, pH=7.4) three times, each time 1mL. Buffer B (20mM PBS, 0.5M sodium chloride, 5mM imidazole, pH=7.4) was washed three times, each time 1mL. Wash with ultrapure water three times, each time 1mL. The material was then copper ion chelated with 0.5 mL of copper chloride solution (0.1 M). Then wash three times with ultrapure water and buffer B respectively. After the supernatant was removed, 0.1 mL of ethanol was added for preservation, and the copper ion chelation column material was obtained.

[0038] The adsorption capacities of the synthesized nano-cuprous sulfide-modified monolithic columns and the commercialized copper...

Embodiment 3

[0045] Example 3: Nano cuprous sulfide modified monolithic column is used for the enrichment of kanamycin sulfate in milk

[0046] Add 10mL of fresh milk purchased from the supermarket, add kanamycin sulfate to make it 1μg / mL, and let it stand for 10 minutes to make it fully effective, add 1.25mL trichloroacetic acid (10%), vortex for 30s, ultrasonic for 15min, centrifuge Take 150 μL of supernatant for LC-MS detection, then take 6 mL of supernatant, add 350 μL of sodium hydroxide (1M) and 4.23 mL of acetonitrile, centrifuge and remove the supernatant for solid phase extraction.

[0047] Take a 3cm monolithic column modified with nano-cuprous sulfide, equilibrate with pH10 buffer, then load 1.5mL of sample, 0.1mL of 90% acetonitrile for weak washing, and then 100μL of eluent (80mM ammonium formate, 0.16% acetic acid, 20% acetonitrile) Eluted and used for LC-MS analysis. Figure 5 The MRM charts were detected for kanamycin sulfate before and after enrichment.

[0048] The mono...

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Abstract

The invention discloses a monolithic column modified by nano cuprous sulfide and a preparation method thereof. Firstly, the hybrid monolithic column skeleton was synthesized, and cuprous oxide nanocubes with a certain thickness were physically adsorbed on its surface, and more stable cuprous sulfide was obtained by treating with sodium sulfide solution, that is, a monolithic column decorated with nano-cuprous sulfide was obtained. The monolithic column obtained by this method has the characteristics of easy fabrication and high permeability of conventional monolithic columns. At the same time, the introduction of nano-cuprous sulfide provides specific adsorption sites, which have strong adsorption for carboxyl, amino and nitrogen heterocyclic structures. Moreover, the specific surface area of ​​the material is significantly increased. The material was prepared into a capillary solid-phase extraction column to realize high-capacity enrichment of kanamycin sulfate in milk under alkaline conditions.

Description

technical field [0001] The invention belongs to the field of liquid chromatography column materials, and in particular relates to a monolithic column modified by nanometer materials and a preparation method thereof. Background technique [0002] Immobilized metal ion affinity chromatography has been widely used in the past few decades for the selective enrichment of biological macromolecules, metabolic and environmental small molecules, among which Cu 2+ , Fe 3+ , Ni 2+ ,Co 2+ , Zr 4+ etc. Different metal ions have different adsorption characteristics. However, metal ions are more sensitive to the pH of the solution, especially in alkaline solution conditions, which will cause metal oxides to precipitate and attach, which will significantly reduce the adsorption capacity. At the same time, strong eluents will easily cause the loss of metal ions. In order to overcome these problems, metal oxide affinity chromatography has been developed, among which nano-zirconia, cerium...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01D15/38
Inventor 许国旺单圆鸿窦阿波石先哲路鑫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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