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Sibutramine magnetic molecularly imprinted polymer and preparation method thereof

A magnetic molecular imprinting and molecular imprinting technology, which is applied to alkali metal compounds, chemical instruments and methods, and other chemical processes, can solve the problems of increased detection costs, high maintenance costs, and high costs, and achieve reduced interference, simple adsorption, The effect of easy operation

Inactive Publication Date: 2014-05-28
NANJING MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The components of natural products in functional foods are complex. In order to eliminate the interference of natural products in functional foods on the detection of illegally added sibutramine, it is necessary to use large-scale instruments such as high-performance liquid chromatography-mass spectrometers that are expensive and high in maintenance costs, which increases the detection the cost of
[0006] Molecularly imprinted polymers have strong specificity and high selectivity, but the adsorption, cleaning, and desorption of molecularly imprinted polymers require methods such as centrifugation, and the separation process is relatively complicated.

Method used

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  • Sibutramine magnetic molecularly imprinted polymer and preparation method thereof
  • Sibutramine magnetic molecularly imprinted polymer and preparation method thereof
  • Sibutramine magnetic molecularly imprinted polymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1: Magnetic nanoparticles (Fe 3 o 4 SiO 2 ) preparation:

[0031] At room temperature, add 80 mL of deoxygenated deionized water into a 250 mL three-neck flask, and keep stirring at 800 rpm min -1 , FeCl was added under the protection of nitrogen 2 4H 2 O (1.72 g) and FeCl 3 ·6H 2 O (4.72 g), when the temperature rises to 80°C, add 10 mL of ammonia water (28%wt) dropwise, react for 1 h, then add 2 mL of PEG-200, stir for 10 min, magnetically separate, wash with deionized water until neutral , that is, Fe 3 o 4 Magnetic nanoparticles, dispersed in isopropanol for later use.

[0032] Take Fe 3 o 4 0.3 g of magnetic nanoparticles was dispersed in 50 mL of isopropanol and sonicated for 15 min. Keep stirring speed 200 rpm min -1 , add 2 mL of deionized water and 2 mL of ammonia water (28%wt), with 20 μL min -1 Add 5 mL of tetraethyl orthosilicate (TEOS) at a high speed, react at room temperature for 12 h, wash with deionized water until neutral, an...

Embodiment 2

[0044] Example 2: Preparation of MMIPs (Method 2)

[0045] With embodiment 1, difference is: take the Fe of functionalization modification 3 o 4 SiO 2 Nanoparticles 40 mg, 1 mmol of (±)N-{1-[1-(4-chlorophenyl)cyclobutyl]-3-methylbutyl}-N-methyl-N-methacrylamide, 3 mmol of functional monomer 4-vinylpyridine was uniformly dispersed in 100 mL of toluene-acetonitrile (9:1, v / v), and stirred at room temperature for prepolymerization for 1 h; then 6 mmol of cross-linking agent trimethylolpropane trimethyl Acrylic ester (TMPTMA) and 80 mg initiator azobisisobutyronitrile (AIBN), nitrogen gas for 15 min to remove oxygen, sealed, heated to 50 °C for 6 h; then heated to 60 °C for 24 h; finally in The reaction was completed at 85°C for 6 h. The resulting MMIPs were separated under an external magnetic field, and then eluted repeatedly with 1M hydrochloric acid solution to remove template molecules, then washed with methanol until neutral, and the polymer was vacuum-dried for later us...

Embodiment 3

[0047] Embodiment 3: selective adsorption test

[0048] Accurately weigh several portions of 20 mg MMIPs and MNIPs and disperse in 10 mL of 2.0 mM sibutramine and its active metabolite M 1 and M 2 Shake the toluene-acetonitrile (9:1, v / v) solution at room temperature for 1 h, then magnetically separate, take the supernatant, and measure the concentration of the sample solution before and after adsorption by HPLC-UV. Concentration change, calculate the adsorption amount of MMIPs and MNIPs to different compounds ( figure 2 ), sibutramine MMIPs (method 2) have a good adsorption effect on sibutramine, sibutramine metabolite M1, and sibutramine metabolite M2, and its adsorption capacity is much larger than that of MNIPs. It shows that sibutramine MMIPs have a specific recognition effect on sibutramine and its metabolite molecules.

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Abstract

The invention discloses a sibutramine magnetic molecularly imprinted polymer and a preparation method thereof. The molecularly imprinted polymer is a magnetic molecularly imprinted polymer having a core-shell structure composed of a core made of Fe3O4@SiO2 magnetic nano particles and a shell made of sibutramine molecularly imprinted polymers. The magnetic molecularly imprinted polymer has special absorption on sibutramine, thus interference of other components on sibutramine detection can be reduced; moreover, the magnetic molecularly imprinted polymer can be directionally controlled by an external magnetic field, thus the absorption, washing, desorption can be conveniently completed, the operation is convenient, so the magnetic molecularly imprinted polymer is suitable for detection of sibutramine illegally added in food and active metabolite of sibutramine namely M1 and M2.

Description

[0001] technical field [0002] The invention belongs to the technical field of molecularly imprinted polymers, and specifically relates to providing an anti-sibutramine and its active metabolite M 1 and M 2 Magnetic molecularly imprinted polymers (MMIPs) with specific recognition. Using this magnetic molecularly imprinted polymer, it is possible to recognize sibutramine and its active metabolite M in a complex environment 1 and M 2 , can be used for the inspection of sibutramine illegally added in functional foods. [0003] Background technique [0004] Sibutramine (Sibutramine) is a central nervous system depressant, which has excitatory and antiemetic effects. However, sibutramine may increase the risk of heart disease and stroke. In 2010, weight-loss drugs containing sibutramine were banned from sale in Europe and the United States. my country also banned the sale and use of sibutramine in 2010. Ingredients of weight loss pills. However, cases of illegal addition o...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08J9/26B01J20/26B01J20/28B01J20/30
Inventor 许贯虹戴鹏赵婷陈云李婷李飞胡琴
Owner NANJING MEDICAL UNIV
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