Zolpidem molecularly imprinted solid-phase extraction columella

A solid-phase extraction cartridge, zolpidem molecule technology, applied in the direction of material separation, analysis of materials, separation methods, etc., can solve the problems of weak specificity, large amount of organic solvent, and more interference of impurities, and achieves auxiliary identification and Detection, high selectivity, high specificity effect

Active Publication Date: 2013-06-05
ACADEMY OF FORENSIC SCIENCE
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the pretreatment methods for zolpidem mainly include liquid-liquid extraction, solid-phase extraction, etc.; "In the article, the liquid-liquid extraction method is used to extract and then analyzed by GC-MS / MS method, but the liquid-liquid extraction method is not specific, there are many impurities, and the amount of organic solvent is large; the solid phase extraction method such as Zhang Leiping, etc. After being extracted by the solid-phase extraction column disclosed in "Solid Phase Extraction-Gas-Phase Extraction Chromatography Analysis of Zolpidem in Whole Blood" (Criminal Technology, No. 2, 2010), the solid-phase Although the phase extraction method has few impurities, its extraction recovery rate is not high, and it is time-consuming and costly

Method used

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  • Zolpidem molecularly imprinted solid-phase extraction columella

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Experimental program
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Effect test

Embodiment 1

[0036] 1mmol zolpidem was dissolved in 10mL chloroform, 4mmol methacrylic acid was added, and placed in a shaker for 1h, so that the template molecules and functional monomers could fully interact.

[0037] Then add 40mmol crosslinking agent ethylene glycol dimethacrylate, 100mg initiator 1,1-dimethyl-1-hydroxyacetophenone, after fully dissolving, transfer the mixed solution into a 50mL ampoule bottle, discharge oxygen, Vacuum tight.

[0038] Place the sealed ampoule in a water bath, irradiate with a 1000W high-pressure mercury lamp for 4 hours, and react to produce a hard solid polymer. Grind and sieve the obtained polymer, collect the polymer with a particle size of 75-125 μm, and pump it in Soxhlet Wash the container with methanol-acetic acid (volume ratio 8:2) until no zolpidem is detected by UV detection, and then wash away the acetic acid with methanol. The polymer was dried under vacuum at 60 °C for 24 h.

[0039] The polymer with a particle size of 75-125 μm was used a...

Embodiment 2

[0046] 1mmol of zolpidem was dissolved in 10mL of chloroform, 8mmol of methacrylic acid was added, and placed in a shaker for 1.5h to make the template molecules fully interact with the functional monomers.

[0047] Then add 100mmol crosslinking agent ethylene glycol dimethacrylate and 100mg initiator diphenyl ethyl ketone, after fully dissolving, transfer the mixed solution into a 50mL ampoule bottle, discharge oxygen, and vacuum seal.

[0048] Place the sealed ampoule in a water bath, irradiate with a 1000W high-pressure mercury lamp for 5 hours, and react to produce a hard solid polymer. Grind and sieve the obtained polymer, collect the polymer with a particle size of 75-125 μm, and pump it in Soxhlet Wash the container with methanol-acetic acid (volume ratio 8:2) until no zolpidem is detected by UV detection, and then wash away the acetic acid with methanol. The polymer was dried under vacuum at 60 °C for 24 h.

[0049] The polymer with a particle size of 75-125 μm was us...

Embodiment 3

[0052] 1mmol of zolpidem was dissolved in 10mL of chloroform, 2mmol of methacrylic acid was added, and placed in a shaker for 1.5h to make the template molecules fully interact with the functional monomers.

[0053] Then add 30mmol crosslinking agent ethylene glycol dimethacrylate, 100mg initiator 2-hydroxyl-2-methyl-1-phenylacetone, after fully dissolving, transfer the mixed solution into a 50mL ampoule bottle, discharge oxygen, Vacuum tight.

[0054] The sealed ampoule was placed in a water bath and irradiated by a 1000W high-pressure mercury lamp for 3.5 hours to produce a hard solid polymer. The obtained polymer was ground and sieved, and the polymer with a particle size of 75-125 μm was collected. Wash with methanol-acetic acid (volume ratio 8:2) in the gas tank until no zolpidem is detected by ultraviolet detection, and then wash away the acetic acid with methanol. The polymer was dried under vacuum at 60 °C for 24 h.

[0055] The polymer with a particle size of 75-125...

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Abstract

The invention provides a preparation method of a zolpidem molecularly imprinted polymer and a zolpidem molecularly imprinted solid-phase extraction columella prepared by the zolpidem molecularly imprinted polymer. Zolpidem is used as template molecules of the zolpidem molecularly imprinted polymer, and the zolpidem molecularly imprinted polymer is obtained by functional monomers and cross-linking agents in a copolymerization mode. The zolpidem molecularly imprinted solid-phase extraction columella comprises a hollow column and zolpidem molecularly imprinted polymer particles filled in the hollow column. The zolpidem molecularly imprinted polymer and the zolpidem molecularly imprinted solid-phase extraction columella prepared by the zolpidem molecularly imprinted polymer are strong in specificity and high in selectivity, the template molecules can be selectively adsorbed from a complex system, separation and concentration can be combined, so that the purpose that separation, purification and quantitative determination are carried out at the same time is achieved, and the zolpidem molecularly imprinted polymer and the zolpidem molecularly imprinted solid-phase extraction columella prepared by the zolpidem molecularly imprinted polymer can be used for detecting practical samples and assisting legal medical experts in identification and detection of zolpidem relative cases in the field of toxicological analysis.

Description

technical field [0001] The invention relates to a tool and method for analyzing pretreatment of zolpidem in biological samples, in particular to an extraction small column and method for pretreatment of zolpidem by solid phase extraction. Background technique [0002] Zolpidem (also known as "Sinuosi"), the chemical name is N,N,6-trimethyl-2-(4-methylphenyl)-imidazo[1,2-a]pyridine-3 -Acetamide, generally made into tartrate, is a new type of non-benzodiazepine sedative and hypnotics with an imidazopyridine structure. It produces pharmacological effects by selectively binding to the ω1-receptor subtype of the central nervous system. For the treatment of short-term insomnia, the blood concentration reaches the peak after 0.5~3h, and the bioavailability is 70%. Because zolpidem has a rapid hypnotic effect and can cause a certain degree of amnesia, it is often used by criminals. In recent years, cases involving zolpidem in forensic toxicology analysis have been on the rise. Comm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285B01J20/30B01D15/22G01N30/88
Inventor 向平施妍沈敏卓先义沈保华
Owner ACADEMY OF FORENSIC SCIENCE
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