A kind of rosin-based bonded silica gel stationary phase and preparation method thereof

A technology of bonding silica gel and rosin base, which is applied in chemical instruments and methods, other chemical processes, alkali metal compounds, etc., can solve the problems affecting the stability of chromatographic columns, the particle size is not particularly uniform, and the thickness of the coating is uncontrollable. Achieve good application prospects, increase space selectivity, and select the effect of separation performance

Active Publication Date: 2021-09-24
GUANGXI UNIV FOR NATITIES +1
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  • Claims
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Problems solved by technology

[0005] The invention patent with application number 201911040979.4 discloses a highly cross-linked rosin-based polymer microsphere and its preparation method and application. Ester is a crosslinking agent, methyl methacrylate is a functional monomer, and highly crosslinked rosin-based polymer microspheres are prepared and used as chromatographic column fillers, which have a good separation effect on total saponins of Panax notoginseng; but its particle size is not Very uniform, relatively high column pressure, which limits its practical application
[0006] The invention patent with application number 201811522372.5 discloses a core-shell SiO 2 @Rosin-based polymer microsphere and its preparation method, which mixes rosin-based crosslinking agent, acrylic monomer and free radical initiator evenly, then evenly coats the surface of silica gel, and then puts it in the water phase for free radical polymerization The reaction yields core-shell SiO 2 @Rosin-based polymer microspheres are used as chromatographic fillers, showing good separation effect on alkaloids, gastrodin and their derivatives; because of the physical coating method, the thickness of the coating is uncontrollable, and the ligand is easy to use during use Bleed, affecting the stability of the chromatographic column

Method used

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  • A kind of rosin-based bonded silica gel stationary phase and preparation method thereof
  • A kind of rosin-based bonded silica gel stationary phase and preparation method thereof
  • A kind of rosin-based bonded silica gel stationary phase and preparation method thereof

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preparation Embodiment 1

[0035] First put 6.0g of silica gel into aqueous hydrochloric acid solution, reflux for 4 hours under the protection of nitrogen, wash with high-purity water until neutral, and dry in vacuum to obtain the activation of silica gel; then 5.0g of activated silica gel, 40.0g of anhydrous toluene, 4.0g of 3 -(methacryloyloxy)propyltrimethoxysilane was added to a three-necked flask, stirred magnetically, refluxed for 4 hours, washed with toluene and acetone, and dried in vacuum to obtain silica gel modified with silane coupling agent; finally, 5.0 g of disproportionated rosin (β- Dissolve acryloyloxyethyl) ester in ethyl acetate, then add 6.0g of silane coupling agent to modify silica gel, disperse by ultrasonic, add 0.05g of initiator azobisisobutyronitrile, protect with nitrogen, and react at 75°C for 4h to obtain Rosin-based bonded silica stationary phase.

preparation Embodiment 2

[0037] First put 11.0g of silica gel into aqueous hydrochloric acid solution, reflux for 3 hours under the protection of argon, wash with high-purity water until neutral, and dry in vacuum to obtain the activation of silica gel; then 10.0g of activated silica gel, 50.0g of anhydrous toluene, 12.0g Add (3-mercaptopropyl) trimethoxysilane into a three-necked flask, stir magnetically, reflux for 6 hours, wash with toluene and methanol, and dry in vacuo to obtain silane coupling agent-modified silica gel; finally, 10.0 g of dehydroabietic acid (β - Dissolve acryloyloxyethyl) ester in butyl acetate, then add 13.0g of silane coupling agent to modify silica gel, disperse by ultrasonic, add 0.1g of initiator dibenzoyl peroxide, and react at 70°C under the protection of argon After 10 h, a rosin-based bonded silica gel stationary phase was obtained.

preparation Embodiment 3

[0039] First put 22.0g of silica gel into aqueous hydrochloric acid solution, reflux for 12h under the protection of nitrogen, wash with high-purity water until neutral, and dry in vacuum to obtain the activation of silica gel; then 20.0g of activated silica gel, 200.0g of anhydrous toluene, 18.0g ( Add 3-mercaptopropyl)triethoxysilane into a three-necked flask, stir magnetically, reflux for 7 hours, wash with toluene and ethanol, and dry in vacuum to obtain silane coupling agent-modified silica gel; In ethyl acetate, add 23.0g silane coupling agent to modify silica gel, ultrasonically disperse, add 0.3g initiator tert-butyl hydroperoxide, and react at 76°C for 8h under nitrogen protection to obtain rosin-based bonded silica gel stationary phase.

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Abstract

The invention discloses a rosin-based bonded silica gel stationary phase and a preparation method thereof, belonging to the technical field of high performance liquid chromatography columns. In the present invention, the activated silica gel is modified with a silane coupling agent, and reacted with a polymerizable rosin-based monomer under the condition of an initiator to form a rosin-based bonded silica gel stationary phase material, and the particle size distribution of the obtained stationary phase material is 2-10 μm , with an average pore diameter of 3‑50nm and a specific surface area of ​​50‑500m 2 / g, and excellent sphericity, uniform particle size, high mechanical strength, and high pressure resistance, it can be used as a chromatographic column packing. The invention also discloses a preparation method of rosin-based bonded silica gel stationary phase. The preparation method is simple, the column pressure is low, and the reproducibility is good. The bonded rosin group has a phenanthrene ring skeleton, which is suitable for steroids, biological Drugs such as bases have good selective separation performance and have good application prospects.

Description

technical field [0001] The invention belongs to the technical field of high-performance liquid chromatography columns, and relates to a rosin-based bonded silica gel stationary phase and a preparation method thereof. Background technique [0002] High-performance liquid chromatography has the characteristics of high selectivity, high sensitivity, and excellent reproducibility, and has been widely used in the fields of chemistry, medicine, food analysis, and environmental testing. The rapid development of modern science and technology has greatly promoted the rapid development of high performance liquid chromatography analysis technology. The HPLC column is the core system of HPLC. The chemical composition of the surface of the chromatographic packing material is the basis for the establishment and development of the HPLC separation mode, and its performance directly affects the separation effect. [0003] At present, liquid chromatography column packing can be divided into ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/28B01J20/30
CPCB01J20/28004B01J20/28061B01J20/28083B01J20/286
Inventor 李浩雷福厚谢文博李文覃丽婷李军
Owner GUANGXI UNIV FOR NATITIES
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