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Preparation of polyacrylamide-coated composite silica gel and application of composite silica gel as chromatographic filler

The technology of polyacrylamide and silica gel is applied in the field of high-performance liquid chromatography separation and analysis, which can solve the problems of complicated preparation process and expensive chromatographic column, and achieve the effects of reducing laboratory cost, excellent separation effect and low preparation cost.

Active Publication Date: 2019-02-22
LANZHOU 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

At present, amino chromatographic columns are commonly used to separate sugar compounds, but such chromatographic columns are relatively expensive, the preparation process is relatively complicated, and a large amount of toxic solvents that are harmful to the human body and the environment are used. Therefore, the development of green and efficient new chromatographic material is necessary

Method used

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  • Preparation of polyacrylamide-coated composite silica gel and application of composite silica gel as chromatographic filler
  • Preparation of polyacrylamide-coated composite silica gel and application of composite silica gel as chromatographic filler
  • Preparation of polyacrylamide-coated composite silica gel and application of composite silica gel as chromatographic filler

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] PAM@SiO 2 The preparation of packing comprises the following steps:

[0024] (1) Silica gel activation: take 8 g of silica gel, heat and reflux with 6 mol / L hydrochloric acid for 4 h, wash with water until neutral, and vacuum dry at 70 °C for 6 h for later use;

[0025] (2) Preparation of polyacrylamide solution: Take 0.2 g of polyacrylamide solid particles with a molecular weight of 10 million, add them to 1000 mL of distilled water, and stir magnetically for 24 h to dissolve them evenly;

[0026] (3) Surface modification and curing of silica gel: Take 5 g of activated silica gel, add it to 150 mL polyacrylamide solution, treat it ultrasonically for 10 min, and then stir it magnetically at 70 °C until the solution evaporates to dryness. Wash once with aqueous solution. The composite microspheres prepared above were dried under vacuum at 70°C for 8 h to cure the polyacrylamide molecules coated on the silica gel surface;

[0027] (5) Polyacrylamide-wrapped composite s...

Embodiment 2

[0028] Embodiment 2, the chromatographic separation of ribose

[0029] PAM@SiO 2 Preparation of chromatographic column: PAM@SiO prepared in Example 1 was prepared by high-pressure homogenization 2 The chromatographic filler is packed into a 150×4.6mm stainless steel liquid chromatographic column for the separation and analysis of sugar compounds. During the filling process, the dispersion liquid is carbon tetrachloride, the displacement liquid is n-hexane, and the pressure is 40 MPa.

[0030] Chromatographic separation of ribose: chromatographic analysis conditions are as follows: mobile phase is 90% acetonitrile aqueous solution; flow rate is 1.0 mL / min; evaporative light scattering detector, gas flow rate is 4 L / min, temperature is 115°C; injection volume is 20 µL .

[0031] The liquid chromatogram of ribose is shown in figure 2 . Under the above chromatographic analysis conditions, the retention time of ribose is 4.3 min, and the column efficiency is about 50000 / m.

Embodiment 3

[0032] Embodiment 3, the chromatographic separation of arabinose

[0033] PAM@SiO 2 Preparation of chromatographic column: PAM@SiO prepared in Example 1 was prepared by high-pressure homogenization 2 The chromatographic filler is packed into a 150×4.6mm stainless steel liquid chromatographic column for the separation and analysis of sugar compounds. During the filling process, the dispersion liquid is carbon tetrachloride, the displacement liquid is n-hexane, and the pressure is 40 MPa.

[0034] Chromatographic separation of arabinose: chromatographic analysis conditions are as follows: mobile phase is 90% acetonitrile aqueous solution; flow rate is 1.0 mL / min; evaporative light scattering detector, gas flow rate is 4 L / min, temperature is 115 °C; 20 µL.

[0035] The liquid chromatogram of arabinose is shown in image 3 . The retention time of arabinose is 6.4 min, and the column efficiency is about 60000 / m.

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Abstract

The invention discloses preparation of polyacrylamide-coated composite silica gel. According to the preparation, a layered physical coating technique is adopted to introduce polyacrylamide linear hydrophilic molecules on the surface of fully-porous spherical silica gel to prepare the multilayer polyacrylamide-coated composite silica gel. Due to excellent hydrophilicity and polarity, polyacrylamidehas strong separation ability for saccharide mixtures under the condition of mobile phase of acetonitrile and water. The composite silica gel can be used as the chromatographic filler for efficient separation of various monosaccharides, disaccharides and polysaccharides. Experiments show that the composite silica gel can achieve rapid baseline separation of more than 10 kinds of oligosaccharidesat the same time, and the column efficiency can be up to more than 150000 / m, so that the separation effect is excellent. The preparation method of the composite silica gel chromatographic filler doesnot involve chemical reaction and addition of toxic reagents, so that the synthesis process is green and environmentally friendly, the preparation cost is relatively low, and the test cost for analysis and detection of saccharide compounds is significantly reduced.

Description

technical field [0001] The invention relates to the preparation of polyacrylamide-wrapped composite silica gel, which is mainly used as a high-performance liquid chromatography filler for the separation of sugar compounds, and belongs to the technical field of high-performance liquid chromatography separation and analysis. Background technique [0002] Excessive intake of sugar compounds will lead to the occurrence of diseases such as obesity and diabetes. With the increasing health awareness of people, more attention is paid to the dosage control of such substances, so accurate detection of sugar compounds is particularly important. The steps of high performance liquid chromatography for the determination of soluble sugar content are relatively simple, without derivatization, and the analysis effect on monosaccharides and oligosaccharides is better. At present, amino chromatographic columns are commonly used to separate sugar compounds, but such chromatographic columns are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281G01N30/02G01N30/06
CPCB01J20/281G01N30/02G01N30/06G01N2030/065
Inventor 王帅王玉环梁晓静郭勇王磊
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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