A kind of sibutramine magnetic molecularly imprinted polymer and its preparation method

A magnetic molecular imprinting and molecular imprinting technology, applied in the directions of alkali metal compounds, chemical instruments and methods, and other chemical processes, can solve the problems of increased detection cost, high maintenance cost, high cost, etc., and achieve simple operation and reduce interference. Effect

Inactive Publication Date: 2016-07-06
NANJING MEDICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] 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
[0004] 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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  • A kind of sibutramine magnetic molecularly imprinted polymer and its preparation method
  • A kind of sibutramine magnetic molecularly imprinted polymer and its preparation method
  • A kind of sibutramine magnetic molecularly imprinted polymer and its preparation method

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Effect test

Embodiment 1

[0025] Embodiment 1: Magnetic nanoparticles (Fe 3 o 4 SiO 2) preparation:

[0026] At room temperature, add 80 mL of deoxygenated deionized water into a 250 mL three-necked bottle, and keep the stirring speed at 800 rpm -1 , FeCl was added under the protection of nitrogen 2 4H 2 O (1.72g) and FeCl 3 ·6H 2 O (4.72g), when the temperature rises to 80°C, add ammonia water (28%wt) 10mL dropwise, react for 1h, then add PEG-2002mL, stir for 10min, magnetically separate, wash with deionized water until neutral, and obtain Fe 3 o 4 Magnetic nanoparticles, dispersed in isopropanol for later use.

[0027] Take Fe 3 o 4 Magnetic nanoparticles 0.3g, dispersed in 50mL isopropanol, ultrasonic 15min. Keep stirring speed 200rmpmin -1 , add deionized water 2mL and ammonia water (28%wt) 2mL, with 20μLmin -1 Add 5 mL of tetraethyl orthosilicate (TEOS) at a high speed, react at room temperature for 12 hours, wash with deionized water until neutral, and dry in vacuum to obtain magneti...

Embodiment 2

[0036] Embodiment 2: the preparation of MMIPs (method 2)

[0037] 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 The functional monomer 4-vinylpyridine was uniformly dispersed in 100mL of toluene-acetonitrile (9:1, v / v), and stirred at room temperature for 1h prepolymerization; then 6mmol of crosslinking agent trimethylolpropane trimethacrylate ( TMPTMA) and 80 mg of initiator azobisisobutyronitrile (AIBN), nitrogen gas was passed for 15 minutes to remove oxygen and then sealed, heated to 50°C for 6 hours; then heated to 60°C for 24 hours; and finally reacted at 85°C for 6 hours. The obtained MMIPs were separated under an external magnetic field, and the template molecules were repeatedly eluted with 1M hydrochloric acid solution to remove template molecules, then washed with methanol until neutral, and the poly...

Embodiment 3

[0038] Embodiment 3: selective adsorption test

[0039] Accurately weigh several portions of 20mg MMIPs and MNIPs dispersed in 10mL of 2.0mM 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 in a constant temperature oscillator, then magnetically separate, take the supernatant, and measure the concentration of the sample solution before and after adsorption by HPLC-UV. According to the concentration of the solution before and after binding , and calculate the adsorption capacity of MMIPs and MNIPs for different compounds ( image 3 ), 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

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 with Fe3O4SiO2 magnetic nanoparticles as the core and sibutramine molecularly imprinted polymer as the shell thing. The magnetic molecularly imprinted polymer prepared by the present invention has specific adsorption on sibutramine, which can reduce the interference of other components on the detection of sibutramine, and more importantly, it can be easily and conveniently controlled by an external magnetic field. Complete adsorption, cleaning, desorption, easy to operate, suitable for the inspection of illegally added sibutramine and its active metabolites M1 and M2 in functional foods.

Description

technical field [0001] 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. Background technique [0002] 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 of sibutramine to fu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08J9/26B01J20/26B01J20/28B01J20/30
Inventor 许贯虹陈明路赵婷吴剑虹李婷李飞胡琴
Owner NANJING MEDICAL UNIV
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