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Solid-phase microextraction probe, preparation method and application of solid-phase microextraction probe in biogenic amine detection

A biogenic amine and extraction technology, applied in chemical instruments and methods, measuring devices, other chemical processes, etc., can solve the problems of unsatisfactory biogenic amine extraction performance, expensive commercial probes, poor mechanical properties, etc., and achieve good extraction efficiency. and mechanical stability, improve mechanical stability and thermal stability, and enhance the effect of adsorption affinity

Active Publication Date: 2022-08-02
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Commonly used commercial probes are expensive, with an average price of about 1,000 yuan per piece. The extraction performance of biogenic amines is not ideal, the mechanical properties are poor, and they are easy to damage

Method used

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  • Solid-phase microextraction probe, preparation method and application of solid-phase microextraction probe in biogenic amine detection
  • Solid-phase microextraction probe, preparation method and application of solid-phase microextraction probe in biogenic amine detection
  • Solid-phase microextraction probe, preparation method and application of solid-phase microextraction probe in biogenic amine detection

Examples

Experimental program
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Effect test

Embodiment 1

[0042] The solid phase microextraction probe of the embodiment of the present invention includes a metal rod and a surface coating coated on the metal rod, and the surface coating is composed of MCM-T-H material and polyacrylonitrile.

[0043] The preparation method of the above-mentioned solid-phase microextraction probe is as follows.

[0044] The above-mentioned MCM-T-H material is obtained by the following method:

[0045] Step S1, synthesis of MCM-41: take 1.25g of hexadecyltrimethylammonium bromide (that is, template molecule, denoted as CTAB) and mix with 490mL of 14% ammonia solution by mass, and uniformly stir at 60°C, Then, tetraethyl silicate (about 10 mL) was added dropwise to the above mixed solution until a white slurry was produced; after 2 hours of reaction, it was cooled, filtered and washed with deionized water for several times; the final product was calcined at high temperature for 12 hours to remove hexadecane Alkyl trimethyl ammonium bromide (that is, remo...

Embodiment 2

[0052] In order to compare the biogenic amine enrichment performance of the solid-phase microextraction probe in Example 1 and the commercial extraction probe. Before gas chromatography detection, the SPE probe was placed in the injection port of the GC-MS instrument for aging at 250 °C for 1 h (ie, heating for 1 h). Take 10mL of concentration as 5mg L -1 , pH=11 biogenic amine standard sample mixed solution in 20mL headspace vial, add 10uL isobutyl chloroformate (ie derivatization reagent), the above-mentioned solid phase microextraction probe or commercial divinylbenzene / Carboxen / Polydimethylsiloxane (DVB / CAR / PDMS) probe (purchased from Supelco, Bellefonte, USA) was placed in the solution, and the auxiliary magnetic stirrer was operated at 1250r min -1 The stirring rate was adsorbed for 30 min, and the reaction was carried out at room temperature. After the reaction, the solid-phase microextraction probe was carefully taken out, and the probe was placed in the GC-MS injec...

Embodiment 3

[0055] Example 3: Using the solid-phase microextraction probe of the present invention to prepare the standard curve of 6 kinds of biogenic amines

[0056] Preparation of biogenic amine standard stock solution: Accurately weigh an appropriate amount of various biogenic amine standard products, put them in 50mL small beakers, and use 0.1mol L -1 The hydrochloric acid solution was dissolved and transferred to a 50mL volumetric flask, the volume was adjusted to the mark, mixed well, and the concentration was 1000mg L -1 (Based on various biogenic amine monomers) standard stock solution, stored in a -20°C refrigerator.

[0057] Preparation of biogenic amine standard mixed use solution: draw 0.25mL of each biogenic amine single-component standard stock solution, place them in the same 50mL volumetric flask, dilute to the mark with pure water, mix well, and prepare a biogenic amine standard mixed use solution (5mgL -1 ).

[0058] Preparation of biogenic amine standard series solu...

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Abstract

The invention discloses a solid-phase microextraction probe, which comprises a metal rod and a surface coating coated on the metal rod, and the surface coating is composed of an MCM-T-H material and polyacrylonitrile. The adsorbent has the advantages of being good in mechanical property and good in biogenic amine adsorption performance. The invention further discloses a preparation method of the solid-phase microextraction probe and application of the solid-phase microextraction probe in biogenic amine detection. And the probe also has the advantages of good mechanical property and good biogenic amine adsorption performance.

Description

technical field [0001] The invention belongs to the technical field of biological amine detection, in particular to a preparation method of a solid-phase microextraction probe and its application in biological amine detection. Background technique [0002] Biogenic amines (BAs) are a general term for a class of biologically active nitrogen-containing organic small molecular compounds, which are mainly formed by the decarboxylation of corresponding amino acids by microorganisms or by aldehydes and ketones under the action of amino acid transaminase. produce. The biogenic amines present in food mainly include tryptamine (TRY), phenethylamine (PHE), putrescine (PUT), cadaverine (CAD), histamine (HIS), tyramine (TYR), spermidine (SPD) ) and spermine (SPM), which are widely found in fermented and smoked meat products. The human body can synthesize some trace amounts of biogenic amines to meet the basic metabolism of the body. However, excessive intake of biogenic amines will ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/32B01J20/28G01N30/14G01N30/02
CPCB01J20/281B01J20/3246B01J20/28011G01N30/14G01N30/02Y02A50/20
Inventor 蓝航镇陈梦飞潘道东
Owner NINGBO UNIV
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