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Solid phase extraction material and its preparation method and application

A solid-phase extraction material and reaction technology, which is applied in chemical instruments and methods, other chemical processes, and the improvement of process efficiency, can solve problems such as uncontrollable proportions, and achieve good hydrophilicity, good hydrophilicity, and economic benefits. high effect

Active Publication Date: 2022-05-17
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, which 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 amphiphilic resin microspheres with A New Aggregation Scheme

Method used

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  • Solid phase extraction material and its preparation method and application
  • Solid phase extraction material and its preparation method and application
  • Solid phase extraction material and its preparation method and application

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 it 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) Prepare white balls with uniform particle size: 10...

Embodiment 2

[0090] Select neutral substances at pH=7: nortriptyline (pKa=9.7), amitriptyline (pKa=9.4), triclosan (pKa=8.1); and acidic substances: buclo 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 appropriate amount of the above-mentioned drugs, dissolve them in methanol to make a 1g / L standard stock solution, and draw appropriate amount of 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 of methanol and cleaning the solid phase extraction material with 5mL of water, pass through the solid phase extraction column, and the column flow rate is controlle...

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) are selected as the selected substances, and the strong anion exchange solid phase prepared in Example 1 is selected 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 appropriate amount of the above-mentioned drugs, dissolve them in methanol to make a 1g / L standard stock solution, and draw appropriate amount of 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 of methanol and cleaning the solid phase extraction material with 5mL of water, pass through the solid phase extraction ...

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Abstract

The invention relates to a solid-phase extraction material, a preparation method and application thereof, and belongs to the field of solid-phase extraction. The preparation method comprises the steps of prepolymerizing monomers N-vinylpyrrolidone and divinylbenzene in the presence of a chain transfer agent, and then adding dropwise to monodisperse seed microparticles. In the emulsion of the spheres, the steps of swelling and reacting to prepare white spheres are further carried out, and the white spheres are subjected to the reaction of introducing functional groups to obtain the solid phase extraction material. The solid phase extraction material prepared by the reaction has good spherical shape, large specific surface area and high ion exchange capacity. The prepared solid-phase extraction material works together with various forces in the process of separating and enriching PPCPs, and the extraction efficiency is high. At the same time, adjusting the pH of the eluent during the elution process can control the ionization degree of the substance or the extraction material. The substances are then selectively separated. The extraction experiment results show that the extraction recovery rate of the prepared solid phase extraction material is basically maintained between 85% and 105%, and acidic, basic, 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 Patents(China)
IPC IPC(8): B01J20/285B01J20/30C08F257/02C08F226/10C08F212/36
CPCB01J20/285C08F257/02C08F226/10C08F212/36Y02P10/20B01J20/261B01J20/3071B01J20/3064C02F1/26B01J20/3078B01J2220/445B01J2220/50
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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