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Solid-phase extraction material as well as preparation method and application thereof

A solid-phase extraction material and reaction technology, used in chemical instruments and methods, other chemical processes, and process efficiency improvements, can solve problems such as uncontrollable proportions, and achieve good hydrophilicity, high economic benefits, and ion exchange capacity. high effect

Active Publication Date: 2022-02-01
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the defect that the proportion of hydrophilic monomer N-vinylpyrrolidone participating in the swelling polymerization reaction cannot be controlled in the traditional seed swelling polymerization technology. By adding a prepolymerization link before the secondary swelling polymerization, the hydrophilic substance Before participating in the final polymerization, N-vinylpyrrolidone has formed a prepolymer micelle with the hydrophobic monomer divinylbenzene, has hydrophobic properties, and can enter the activator dibutyl phthalate ( DBP), and then make the hydrophilic substance N-vinylpyrrolidone fully participate in the final polymerization reaction, realize the sufficient polymerization of the hydrophilic monomer N-vinylpyrrolidone and divinylbenzene, and provide the amphiphilic resin microspheres A New Aggregation Scheme

Method used

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  • Solid-phase extraction material as well as preparation method and application thereof
  • Solid-phase extraction material as well as preparation method and application thereof
  • Solid-phase extraction material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080](1) Preparation of monodisperse seed microspheres: Mix 15 mL of ethanol and 15 mL of water as the water phase, add 0.4 g of dispersant polyvinylpyrrolidone and 0.1 g of initiator benzoyl peroxide into the water phase, and stir at 60 ° C for 30 Minutes until completely dissolved; mix 8g styrene and 2g divinylbenzene as the oil phase and add dropwise to the aqueous solution. After mixing evenly, gradually increase the temperature to 75°C at a rate of 3°C every 10 minutes, and keep the stirring rate at 450-500rpm After reacting for 4 hours, monodisperse seed microspheres with a particle size of 5-10 μm were obtained;

[0081] Add 0.5g dispersant polyvinylpyrrolidone, 0.375g emulsifier sodium lauryl sulfate, 2g above-mentioned monodisperse seed microspheres, 10g porogen toluene, 10g swelling agent dimethyl phthalate in 100mL aqueous solution, Emulsion A was prepared through 200W ultrasonic enhanced dispersion;

[0082] (2) Preparation of white balls with uniform particle si...

Embodiment 2

[0090] Select neutral substances under the condition of pH=7: nortriptyline (pKa=9.7), amitriptyline (pKa=9.4), triclosan (pKa=8.1); and acidic substances: Buluo Fen (pKa=4.9), bezafibrate (pKa=3.6), and indomethacin (pKa=4.5) were selected as the selected substances, and the strong cation exchange solid phase extraction material prepared in Example 1 was selected: MAX.

[0091] (1) Fill 500mg of solid-phase extraction material into a 6mL solid-phase extraction column with sieve plates at both ends, weigh an appropriate amount of the above-mentioned drugs, dissolve them in methanol to make a 1g / L standard stock solution, and draw an appropriate amount of the standard stock solution to prepare Prepare a mixed standard solution of 1mg / L, and at the same time make a mixed internal standard solution of 1mg / L.

[0092] (2) After activating with 5mL methanol and cleaning the solid-phase extraction material with 5mL water, pass through the solid-phase extraction column, and the colum...

Embodiment 3

[0096] Select neutral substances under the condition of pH=7: acetaminophen (pKa=9.4), triclosan (pKa=8.14), amphoteric substances: ofloxacin (pKa=5.97, 9.28) and Alkaline substances: clarithromycin (pKa=9.0), erythromycin (pKa=8.9), omeprene (pKa=7.11) as selected substances, choose the strong anion exchange solid phase prepared in Example 1 Extraction material: MCX.

[0097] (1) Fill 500mg of solid-phase extraction material into a 6mL solid-phase extraction column with sieve plates at both ends, weigh an appropriate amount of the above-mentioned drugs, dissolve them in methanol to make a 1g / L standard stock solution, and draw an appropriate amount of the standard stock solution to prepare Prepare a mixed standard solution of 1mg / L, and at the same time make a mixed internal standard solution of 1mg / L.

[0098] (2) After activating with 5mL methanol and cleaning the solid-phase extraction material with 5mL water, pass through the solid-phase extraction column, and the column...

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Abstract

The invention relates to a solid-phase extraction material and a preparation method and application thereof, and belongs to the field of solid-phase extraction. The preparation method comprises the steps that monomers N-vinyl pyrrolidone and divinylbenzene are pre-polymerized in the presence of a chain transfer reagent and then dropwise added into an emulsion of monodisperse seed microspheres, then swelling and reacting are conducted, and white spheres are prepared; the white spheres are subjected to a reaction of introducing functional groups, and the solid-phase extraction material is obtained. The solid-phase extraction material prepared by the reaction is good in spheroidizing morphology, large in specific surface area and high in ion exchange capacity. According to the prepared solid-phase extraction material, in the process of separating and enriching PPCPs, various acting forces jointly play a role on substances, the extraction efficiency is high, meanwhile, the ionization degree of the substances or the extraction material can be controlled by adjusting the pH value of eluent in the elution process, and then the substances are selectively separated. Extraction experiment results show that the extraction recovery rate of the prepared solid-phase extraction material to substances is basically maintained between 85% and 105%, and acidic, alkaline, neutral and amphoteric substances can be selectively separated.

Description

technical field [0001] The invention belongs to the field of solid-phase extraction, and in particular relates to a preparation method and application of a series of enhanced solid-phase extraction materials with uniform particle diameters. Background technique [0002] The performance of the solid phase extraction packing is the key to the extraction efficiency. The functional groups contained in the solid phase extraction packing can realize the enrichment of the compound through the force. The solid phase extraction packing can be divided into molecular polymer matrix, bonded silica gel, inorganic Metal oxides and other enhanced solid-phase extraction packings, among which the enhanced solid-phase extraction packing has multiple functional groups, which can realize the extraction of compounds with multiple forces, making its application range wider than that of single-functional solid-phase extraction columns. wide. Enhanced sorbents extract analytes based on their inter...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/30C08F257/02C08F226/10C08F212/36
CPCB01J20/285C08F257/02C08F226/10C08F212/36Y02P10/20
Inventor 周庆张子昂陈军霞陈禹融雷冲天王冉秋周伟伟章礼斌
Owner NANJING UNIV
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