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Intelligent response liquid chromatogram filling material and preparation method thereof

A liquid chromatography, intelligent technology, applied in the field of intelligent response liquid chromatography packing and its preparation, to achieve the effect of good physical and chemical stability and high mechanical strength

Inactive Publication Date: 2016-05-04
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of this, the object of the present invention is to provide an intelligent response liquid chromatography filler and its preparation method, which can overcome the defects of existing commodity liquid chromatography fillers, and thus be used for the separation of complex samples. This filler is Prepared by encapsulating smart responsive materials on the surface of silica gel via free radical-initiated copolymerization

Method used

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  • Intelligent response liquid chromatogram filling material and preparation method thereof
  • Intelligent response liquid chromatogram filling material and preparation method thereof
  • Intelligent response liquid chromatogram filling material and preparation method thereof

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Embodiment 1

[0036] The specific steps of compounding intelligent response materials on the surface of silicon spheres are as follows:

[0037] (1) Weigh the particle size of 2 ~ 5μm, the pore size is 2g of silicon spheres, mixed with 120mL, 1mol / L HCl ultrasonically, stirred and refluxed at 90°C for 3h, after the reaction, filtered, washed with pure water until neutral, and the washed silicon spheres were heated at 150°C Dry overnight;

[0038] (2) Weigh 1.2 g of the cleaned silicon spheres, suspend them with 50 mL of toluene, add 0.54 mL (3 mmol) of 3-aminopropyltrimethoxysilane (APTES) and react at 20-25 °C for 16 hours, centrifuge in toluene 3 times, suspend again with 50mL toluene, add 0.24mL (3mmol) pyridine, keep it at 0°C in the low temperature reactor, pipette 0.37mL (3mmol) of bromoisobutyryl bromide and dilute with 5mL toluene, under the protection of nitrogen Make it dropwise into the reaction bottle, react at 0°C for 2h, react at room temperature for 12h, wash with toluene,...

Embodiment 2

[0056] (1) The particle size is 6-10 μm and the pore size is 2g of silicon spheres, mixed with 120mL, 5mol / L HCl ultrasonically, stirred and refluxed at 100-110°C for 7h, after the reaction, filtered, washed with pure water until neutral, so that the washed silicon spheres Dry overnight at 150°C;

[0057] (2) Weigh 5 g of the cleaned silicon spheres, suspend them with 80 mL of toluene, add 0.64 mL (4 mmol) of 3-aminopropyltrimethoxysilane (APTES) and react at 90 ° C for 5 h, centrifuge 3 times in toluene, Ultrasonic suspend again with 50mL of toluene, add 0.32mL (4mmol) of pyridine, keep it at 0°C in the low-temperature reactor, pipette 0.37mL (3mmol) of bromoisobutyryl bromide and dilute with 5mL of toluene, and let it drop under the protection of nitrogen Add it into a reaction bottle, react at 0°C for 3 hours, and react at room temperature for 18 hours, wash with toluene, water, methanol, dichloromethane, acetone, and then vacuum dry at 150°C for 2 hours;

[0058] (3) So...

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Abstract

The invention discloses an intelligent response liquid chromatogram filling material. The filling material is made by wrapping silicon balls with an intelligent response material, and the intelligent response material is co-polymer of N-isopropyl acrylamide, 4-(trifluoromethyl)-phenylthiourea-2-acrylamide and 3-acrylamide phenylboronic acid. The filling material can achieve the effect that the intelligent response material is switched from the super hydrophilicity to the super-hydrophobicity through excitation by way of one or more of the temperature, the pH value and carbohydrate so that and the the synthesized filling material can achieve the separation mode of reversion phase chromatography and hydrophilic chromatography of hydrophobic substances, hydrophilic substances and other substances through control over such conditions as the temperature, the pH value and sugar. The invention further discloses a preparation method of the intelligent response liquid chromatogram filling material.

Description

technical field [0001] The invention belongs to the technical field of high performance liquid chromatography packing materials, and in particular relates to an intelligent response liquid chromatography packing and a preparation method thereof. Background technique [0002] High performance liquid chromatography is a widely used analytical chromatographic technique with applications in the fields of biology, chemistry, and pharmaceuticals. Commonly used liquid chromatography modes include normal phase liquid chromatography, reversed phase liquid chromatography, ion exchange liquid chromatography and hydrophilic interaction liquid chromatography. These classic single LC separation modes have encountered challenges in the analysis of complex samples. For example, in the analysis of biological samples, environmental pollutants, and traditional Chinese medicine extracts, their components are complex and their physical and chemical properties vary greatly. Multiple chromatograp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285C08F292/00C08F220/54C08F220/58C08F230/06B01J20/30
CPCB01J20/285B01J2220/46B01J2220/54C08F292/00C08F220/54
Inventor 魏为力王路军夏之宁张欢
Owner CHONGQING UNIV
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