Molecular imprinting material as well as preparation method and application thereof

A technology of molecular imprinting and template molecules, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve the problems of more interference in the detection process, lack of professional materials, etc., to reduce the use of organic solvents, The effect of small particle size and uniform distribution

Inactive Publication Date: 2010-06-09
JIANGSU POLICE INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nowadays, methods such as chemically bonded phase silica gel and macroporous adsorption resin for liquid-solid extraction, solid-phase microextraction membrane for adsorption, organic solvent ethyl acetate direct extraction, and solid-phase microextraction for direct adsorption and sample injection are commo

Method used

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  • Molecular imprinting material as well as preparation method and application thereof
  • Molecular imprinting material as well as preparation method and application thereof
  • Molecular imprinting material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 1mmol template molecule triazolam, 4mmol (0.3443g) a-methacrylic acid, 20mmol (3.9644g) ethylene glycol dimethacrylate to a 100mL three-necked flask successively, let it stand for 12h, and then add a mass concentration of 4 50 mL of dispersant PVA1750, 5 mL of porogen toluene and 0.04 g of AIBN were stirred and reacted for 24 hours at a constant temperature of 65° C. in a water bath at a stirring speed of 300 rpm.

[0032] Wash the obtained microparticles with methanol:acetic acid with a volume ratio of 7:3 in a Soxhlet extractor for 3 times, and the volume of the mixed solution is 10 times the mass of the microparticles, and detect with GC until no triazolam can be detected. until. Then wash with distilled water 4 times to pH 6.9.

[0033] The obtained microparticles were vacuum-dried at 50°C, and the obtained microparticles (100-250 μm) were the desired triazolam molecularly imprinted materials (see attached figure 1 ).

[0034] Take 4 mL of urine and add 2 mg ...

Embodiment 2

[0036]Add 1mmol template molecule, 6mmol (0.426g) acrylamide, 10mmol (1.300g) 1,4-divinylbenzene to a 100mL three-necked flask in sequence, let stand for 12h, then add 50mL of 0.5% dispersant PVA1788, Add 15 mL of chloroform and 0.4 g of AIBN, and stir the reaction for 30 h at a constant temperature of 75 °C in a water bath at a stirring speed of 150 rpm.

[0037] Wash the obtained microparticles with methanol:acetic acid with a volume ratio of 7:3 in a Soxhlet extractor for 5 times. until. Then wash with distilled water 4 times to pH 6.8.

[0038] The obtained microparticles were vacuum-dried at 50°C, and the obtained microparticles (150-200 μm) were the required triazolam molecularly imprinted materials (see attached figure 2 ).

[0039] Take 4 mL of urine and add 2 mg of triazolam. Adjust the pH to 9 with sodium hydroxide solution, put in 0.1000g triazolam molecularly imprinted material (MIPs), absorb at 35°C for 4 hours, filter out the MIPs, add 2 mL of chloroform to ...

Embodiment 3

[0041] Add 1mmol template molecule, 8mmol (0.6886g) a-methacrylic acid, 15mmol (5.070g) trimethylolpropane trimethacrylate to a 100mL three-necked flask in sequence, let it stand for 12h, and then add 2% dispersant PVA1799 50mL, porogen chloroform 50mL and 0.04g AIBN were stirred and reacted at a constant temperature of 65°C in a water bath at a stirring speed of 350 rpm for 24h.

[0042] The obtained microparticles were refluxed and washed 4 times in a Soxhlet extractor with methanol:acetic acid with a volume ratio of 7:3. until. Then washed twice with distilled water to pH 6.5.

[0043] The obtained microparticles were vacuum-dried at 60°C, and the obtained microparticles (20-180 μm) were the desired triazolam molecularly imprinted materials (see attached image 3 ).

[0044] Take 4 mL of urine and add 2 mg of triazolam. Adjust the pH to 9 with sodium hydroxide solution, put in 0.1000g triazolam molecularly imprinted material (MIPs), absorb at 25°C for 4 hours, filter ou...

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Abstract

The invention relates to molecular imprinting material as well as preparation method and application thereof. The method comprises the following steps of: adding a template molecule, a functional monomer and a cross-linking agent into a container according to a proportion and then standing; adding a dispersing agent; finally adding an initiating agent and a hole-inducing agent into the container according to a proportion, controlling the temperature to react and obtaining a microparticle with the particle diameter ranging between 20 microns and 350 microns; refluxing and washing the obtained microparticle by a mixed solution of methanol/acetic acid in the container and detecting by GC (gas chromatography) till triazolam is not detected; washing by distilled water to neutrality; and drying in vacuum to constant weight to obtain the microparticle which is the needed triazolam molecular imprinting material. The prepared imprinting material can be directly used for enriching and separating the triazolam in urine, reduces the dosage of an organic solvent used when the triazolam is extracted by a liquid-liquid extracting method and is beneficial to the body health of an operator. The method does not need the protection of an inert gas, and the compounded material has the characteristics of small particle diameter and uniform distribution.

Description

technical field [0001] The invention relates to the technical field of criminal science, and relates to a molecularly imprinted material and its preparation method and application, in particular to the preparation of triazolam molecularly imprinted and its application to the enrichment and separation of triazolam in urine. Background technique [0002] Triazolam (Triazolam, Halcion) is a benzodiazepine drug developed by Upjohn Company of the United States. It is a psychotropic drug that acts on the benzodiazepine receptor (BZR) of the central nervous system. , because of its fast oral absorption, quick effect, good hypnotic effect, and faster clearance from the body than other similar drugs, it was once praised as one of the most ideal sleeping pills. It is currently listed as the first category of psychotropic drug management by the State Food and Drug Administration. It is clinically used to treat various types of insomnia, recurrent insomnia, and patients who need sleep a...

Claims

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Application Information

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IPC IPC(8): C08F220/06C08F220/56C08F222/14C08F212/36C08F2/44C08J9/26B01D15/00
Inventor 王军王虹周亚红朱斌
Owner JIANGSU POLICE INST
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