Melamine-modified solid-phase extraction agent and solid-phase extraction method for enriching aristolochic acid

A solid-phase extraction agent, aristolochic acid technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problem that molecularly imprinted polymer solid-phase extraction agents cannot be used to enrich molecules, and the enrichment and separation effects are not obvious , Aristolochic acid and other problems have not been seen yet, achieving good specific recognition, avoiding uneven polymerization, and using less solvent

Active Publication Date: 2021-08-13
XI AN JIAOTONG UNIV
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  • Abstract
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Problems solved by technology

Existing solid-phase extraction agents such as C18, C8, and silica gel can be used for sample pretreatment of most substances, which lack selectivity for specific molecules, and the enrichment and separation effect is not obvious; ion-exchange solid-phase extraction agents can be used for weak acids or weak bases However, the molecularly imprinted polymer used for solid-phase extraction has the problem of easy leakage of residual template molecules, and its preparation process It is easily limited by the physical and chemical properties of template molecules such as solubility, and using toxic substances such as aristolochic acid as template molecules will cause harm to the experimenter
At the same time, due to the high specificity of recognition, objectively, the molecularly imprinted polymer solid-phase extraction reagent prepared with a specific template molecule cannot be used to enrich other molecules with similar structures.
However, there has been no report on obtaining a solid-phase extraction agent capable of enriching aristolochic acid through surface modification.

Method used

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  • Melamine-modified solid-phase extraction agent and solid-phase extraction method for enriching aristolochic acid
  • Melamine-modified solid-phase extraction agent and solid-phase extraction method for enriching aristolochic acid
  • Melamine-modified solid-phase extraction agent and solid-phase extraction method for enriching aristolochic acid

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Experimental program
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Effect test

Embodiment 1

[0039] (1) Carboxyl modification of graphite

[0040] Weigh 500 mg of graphite powder (45-150 μm), add it to 50 mL of methanol, and ultrasonically disperse the graphite evenly, then add 170.5 μL of MAA, 376.5 μL of EDMA (the molar ratio of MAA to EDMA is 1:1) and 14 mg of AIBN to the graphite dispersion system , ultrasonically dissolved and mixed evenly, nitrogen was introduced to remove oxygen, sealed and then stirred and polymerized in a 60°C water bath for 12 hours, after filtration, the polymerized product was washed with water and absolute ethanol in sequence to remove unreacted MAA and EDMA, and dried at 50°C to obtain Carboxyl modified graphite.

[0041] (2) Preparation of melamine-modified graphite

[0042] Use the EDC / DMAP reaction system to introduce the amino group and the conjugated system on the carboxyl-modified layer: add 12.6mg of melamine, 92mg of EDC and 9.8mg of DMAP to the 20mL of DMF taken from the vector, and dissolve and mix them by ultrasonic to obtain...

Embodiment 2

[0047] (1) Carboxyl modification of MOF-199

[0048] Weigh 500 mg of MOF-199 (10-30 μm), add it into 50 mL of methanol, and ultrasonically disperse MOF-199 evenly, add 170.5 μL of MAA and 376.5 μL of EDMA to the MOF-199 dispersion in turn (the molar ratio of MAA to EDMA is 1: 1) and 14mg of AIBN, ultrasonically dissolved and mixed, passed through nitrogen to remove oxygen, sealed and stirred in a water bath at 60°C for 12h, after filtration, the polymer product was washed with water and absolute ethanol in order to remove unreacted MAA and EDMA, 50 C and dried to obtain carboxyl-modified MOF-199.

[0049] (2) Preparation of melamine-modified MOF-199

[0050] Use the EDC / DMAP reaction system to introduce the amino group and the conjugated system on the carboxy-modified layer: add 12.6 mg of melamine, 92 mg of EDC and 9.8 mg of DMAP to 20 mL of DMF taken as a vector, and dissolve and mix them by ultrasonic to obtain a reaction solution; weigh the carboxy-modified MOF-199 200 m...

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Abstract

The invention discloses a melamine-modified solid-phase extraction agent and a solid-phase extraction method for enriching aristolochic acid. Using methacrylic acid as the functional monomer to carry out carboxylation modification on the surface of the carrier, adopting EDC / DMAP reaction system to graft melamine on the carboxyl modification layer to obtain a melamine-modified solid with high adsorption capacity and good specific recognition effect. phase extraction agent; the obtained melamine modified solid phase extraction agent is used to prepare a solid phase extraction column, which can be used for selective enrichment and separation of aristolochic acid, combined with high performance liquid chromatography, it can be used for the detection of trace aristolochic acid in traditional Chinese medicine, And it can effectively reduce the interference of other components in the traditional Chinese medicine on the analysis and detection. The preparation method of the solid-phase extraction agent is simple, and can avoid the harm of the template molecule to the experimenter and avoid the impact on the detection caused by the leakage of the template molecule during use.

Description

technical field [0001] The invention relates to material surface modification, in particular to a melamine-modified solid-phase extraction agent and a method for enriching and detecting trace amounts of aristolochic acid in traditional Chinese medicine by using the melamine-modified solid-phase extraction agent. Background technique [0002] Aristolochic acid is a series of nitrophenanthrene acids, widely present in Aristolochiaceae plants such as Aristolochia and Asarum, and is the main active ingredient of Aristolochiaceae plants. Most of the plants in Aristolochiaceae have the functions of clearing the lung and lowering qi, relieving cough and asthma, dispelling wind and relieving pain, regulating qi and relieving pain, and are often used as Chinese herbal medicine for the treatment of arthritis and rheumatism. However, aristolochic acid has nephrotoxic, carcinogenic and mutagenic effects, and can cause renal tubular degeneration, atrophy, necrosis, oligocellular renal in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30C08F220/06C08F222/14
CPCB01J20/286B01J20/3085C08F220/06C08F222/102
Inventor 傅强舒花陈国宁王璐崔霞李璇汪群常春
Owner XI AN JIAOTONG UNIV
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