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Preparation method and application of sulphonamide molecular-imprinting solid-phase extraction columella

A technology for solid-phase extraction small column and sulfonamide drugs, which is applied in the field of analytical chemistry and achieves the effects of low production cost, high separation efficiency and recovery rate, and large adsorption capacity

Inactive Publication Date: 2013-09-11
HUAZHONG AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to overcome the deficiency of existing solid-phase extraction method, is to provide a kind of preparation method of sulfonamide drug molecularly imprinted solid-phase extraction column, this solid-phase extraction column has specificity compared with existing solid-phase extraction column Strong stability, high recovery rate, simple preparation, low cost, easy realization of required instruments and reaction conditions, etc.

Method used

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  • Preparation method and application of sulphonamide molecular-imprinting solid-phase extraction columella
  • Preparation method and application of sulphonamide molecular-imprinting solid-phase extraction columella
  • Preparation method and application of sulphonamide molecular-imprinting solid-phase extraction columella

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1: Preparation of Sulfamethazine Imprinted Polymer

[0036] 1.1. Preparation of Sulfamethazine Imprinted Polymer - Method 1

[0037] First, carry out pre-polymerization, weigh 0.5 mmol of the template molecule (sulfamethazine), add 2 mmol of the functional monomer MAA and dissolve it in acetonitrile, sonicate for 5 minutes and put it in a refrigerator at 4°C for 24 hours to form a stable complex to complete the pre-polymerization. Add cross-linking agent EGDMA 10mmol subsequently, initiator AIBN 0.37mmol, place in the quartz test tube of 18mm * 180mm after sonication 5min and pass nitrogen 5min (remove oxygen), seal under nitrogen atmosphere, put 0 ℃ of ice-water baths, in The polymerization was initiated under a 365nm, 6w ultraviolet lamp, the distance between the ultraviolet lamp and the quartz test tube was 3cm, and the reaction time was 48h. After the reaction, a white blocky polymer was obtained. After grinding it, settle it with acetone for 3 to 5 times, ...

Embodiment 2

[0045] Example 2. Characterization of Sulfamethazine Imprinted Polymers

[0046] 2.1 Characterization of preparation of sulfamethazine imprinted polymer by method 1

[0047] Using the acetonitrile solution of template molecules as the adsorption solution, accurately weigh 10 parts of 50 mg template molecularly imprinted polymers, measure their adsorption capacity for different concentrations of template molecules at 25°C, and plot the adsorption capacity against the concentration of template molecules. Adsorption isotherm curve. In order to compare the adsorption properties of template molecularly imprinted polymers, the isotherm adsorption curves of non-template molecularly imprinted polymers should also be determined at the same time, and the obtained data are used for the Scatchard analysis of formula (1) (see Figure 7 and Figure 8 ). The Q of MIPs can be obtained from the slope and intercept of the Scatchard curve max and K D . The characterization results show tha...

Embodiment 3

[0054] Example 3. Preparation of Molecularly Imprinted Solid Phase Extraction Column

[0055] 3.1 Preparation of Molecularly Imprinted SPE Columns Using Sulfamethazine Imprinted Polymer Prepared by Method 1

[0056]The column packing homogenate was 5 mL of methanol-isopropanol mixture (V / V, 3:1), and 120 mg of template molecularly imprinted polymer or non-template molecularly imprinted polymer were put into the homogenate and sonicated for 5 minutes to prepare a mixed solution. Suspension. Before loading the column, first put the lower sieve plate in, rinse the 3mL SPE empty column tube with 3mL-5mL methanol, then put it on the solid phase extraction vacuum device, seal the empty interface, turn on the vacuum pump, Make the vacuum degree reach -25Pa, add the imprinted polymer suspension that has been homogenized, tap the cylinder gently while adding, put the homogenate into the upper sieve plate and press it tightly before the homogenate is quickly drained. Rinse with 10mL o...

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Abstract

The invention discloses a preparation method and application of sulphonamide molecular-imprinting solid-phase extraction columella. The preparation method comprises the following steps of: (1) mixing a template molecule, a functional monomer and a cross-linking agent; (2) representing molecular-imprinting polymer particles; (3) filling the molecular-imprinting polymer particles into a solid-phase extraction columella, wetting and washing by using methanol and acetone, sealing in vacuum, wherein the sulphonamide molecular-imprinting polymer is obtained by the following steps of: (a) dissolving the template molecule sulfanilamide and the functional monomer in pore-foaming agent acetonitrile to obtain a mixed solution; (b) carrying out ultrasonic treatment onto the mixed solution by an ultrasonic cleaner to obtain a pre-polymerization system; (c) transferring the pre-polymerized system to a quartz reaction test tube, adding cross-linking agent and imitator; (d) placing the pre-polymerization system under ultraviolet light; (e) directly grinding the imprinted polymer to obtain the imprinted polymer particles. The preparation method of the sulphonamide molecular-imprinting solid-phase extraction columella is high in recovery rate, simple to prepare, low in cost and capable of being directly used for selective adsorption and efficient enrichment of sulfadiazine, sulfamerazine and sulfadimidine in animal-origin food.

Description

technical field [0001] The present invention relates to the field of analytical chemistry, more specifically to a method for preparing a small column for molecularly imprinted solid phase extraction of sulfonamide drugs, and also relates to the application of the small column for molecularly imprinted solid phase extraction of sulfonamide drugs, especially for sulfadiazine in animal foods , Sulfamethazine and Sulfamethazine residue analysis in the separation and enrichment of samples. Background technique [0002] Sulfonamides are a class of chemical antibacterial drugs used to prevent bacterial and protozoal infections. This type of drug is a slow antibacterial agent, which can produce adverse reactions such as obvious nephrotoxicity, bone marrow suppression, and rash. Because of its low price and wide antibacterial spectrum, it is widely used in animal husbandry at present, but its abuse and misuse are gradually increasing, resulting in the residues of sulfonamides in ani...

Claims

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Application Information

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IPC IPC(8): C08F220/06C08F220/56C08F226/06C08F220/10C08F222/14C08J9/26B01J20/30B01J20/285G01N30/08
Inventor 袁宗辉李兆周彭大鹏王玉莲陶燕飞黄玲利陈冬梅戴梦红刘振利
Owner HUAZHONG AGRI UNIV
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