Method for preparing benzodiazepine molecule surface blotting solid-phase extractant

A solid-phase extraction agent and surface imprinting technology, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve the leakage of template molecules, unsatisfactory mass transfer rate, and affect the accurate quantification of trace analytes Detection and other problems, to achieve the effect of eliminating the interference of impurities, good selection of adsorption and separation capabilities, and not easy to fragment

Inactive Publication Date: 2009-09-16
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis methods used are generally bulk polymerization and precipitation polymerization. Many binding sites are wrapped in the rigid structure of molecularly imprinted polymers, resulting in unsatisfactory mass transfer rates for selective adsorption of target molecules, and it is difficult for template molecules to be completely removed from the polymer. After elution, leakage of template molecules occurs in actual use, which seriously affects the accurate quantitative detection of trace analytes
[0005] Currently, literature on sol-gel-surface molecularly imprinted polymers has been reported, but no benzodiazepine A report on the related technology of preparing drug-like templates and imprinting polymers on its surface by sol-gel method

Method used

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  • Method for preparing benzodiazepine molecule surface blotting solid-phase extractant
  • Method for preparing benzodiazepine molecule surface blotting solid-phase extractant
  • Method for preparing benzodiazepine molecule surface blotting solid-phase extractant

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Dissolve 0.19g of estazolam in 5mL of methanol, then add 1mL of γ-aminopropyltriethoxysilane, 1.1mL of phenyltrimethoxysilane, stir for about 0.5 hours, add 2mL of tetraethoxysilane, and then Stir for 5 minutes, add 0.5 g of activated silica gel (amorphous, particle size 19-37 μm), and finally add 1 mL of water and adjust the pH to 3 with hydrochloric acid to catalyze hydrolysis and condensation. After the above mixed solution was fully stirred, it was allowed to stand still for about 24 hours to completely hydrolyze and condense, then filtered, and vacuum-dried at 100°C to constant weight. The template molecules were removed by Soxhlet extraction with acetic acid / methanol (1:9, V / V) solution, and then the residual acetic acid on the surface molecularly imprinted polymer was removed with methanol, and finally, vacuum-dried at 80°C for further use.

[0024] figure 1 and 2 They are the SEM images of the solid phase extraction agent synthesized in Example 1 enlarged 500 ...

Embodiment 2

[0028] Dissolve 0.62g of estazolam in 15mL of methanol, then add 1mL of γ-aminopropyltrimethoxysilane, 0.8mL of phenyltrimethoxysilane, stir for about 1 hour, add 4mL of tetramethoxysilane, and then stir For 5 minutes, add 1.8 g of activated silica gel (spherical type, particle size 5-10 μm), and finally add 1 mL of water and adjust the pH to 4 with hydrochloric acid to catalyze the hydrolysis and condensation. After the above mixed solution was fully stirred, it was allowed to stand still for about 12 hours to completely hydrolyze and condense, then filtered, and vacuum-dried at 90°C for 8 hours. The template molecule was removed by Soxhlet extraction with acetic acid / acetonitrile (1:9, V / V) solution, and then the residual acetic acid on the surface molecularly imprinted polymer was removed with methanol, and finally, vacuum-dried at 60°C for use.

[0029] The microsphere solid-phase extraction agent prepared by the above method is used to process biological samples. The expe...

Embodiment 3

[0032] Dissolve 0.27g of diazepam in 15mL of methanol, then add 1mL of γ-aminopropyltriethoxysilane, 1mL of phenyltriethoxysilane, stir for about 0.5 hours, add 4mL of tetraethoxysilane, and then stir for 5 minutes , add 1.8g of activated silica gel (spherical, particle size 5-10μm), and finally add 2mL of water and adjust the pH to 5 with hydrochloric acid to catalyze the hydrolysis condensation. After the above mixed solution was fully stirred, it was allowed to stand still for about 24 hours to completely hydrolyze and condense, then filtered and vacuum dried at 110°C for 8 hours. The template molecule was removed by Soxhlet extraction with acetic acid / methanol (1:9, V / V) solution, and then the residual acetic acid on the surface molecularly imprinted polymer was removed with methanol / ethanol, and finally, vacuum-dried at 80°C for further use.

[0033] In order to prove that the prepared microsphere solid-phase extraction agent has selective adsorption to template molecules...

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Abstract

The preparation method of the surface imprinted solid-phase extractant of benzodiazepine-like molecules comprises firstly dissolving the benzodiazepine-like template molecules in methanol, then adding functional monomer A and functional monomer B, stirring and pre-acting to obtain a prepolymer, Add tetramethoxysilane or tetraethoxysilane to the above solution, stir evenly, then add silica gel particles activated by methanesulfonic acid solution, add acid to catalyze hydrolysis condensation, filter and dry to obtain the crude product, and finally elute and purify the crude product. The preparation process of the method is simple, and the prepared surface molecular imprinted solid-phase extraction agent has selective recognition for target molecules, can completely eliminate the interference of impurities in samples, has high mechanical strength, stable physical and chemical properties, and small swelling coefficient.

Description

1. Technical field [0001] The present invention relates to a kind of benzodiazepine The preparation method of the molecularly imprinted solid-phase extraction agent of class drug, promptly combines sol-gel method and surface imprinting technology, prepares a kind of p-benzodiazepine Drug-like organic-inorganic hybrid solid-phase extraction materials with selective recognition. The extractant is applied to the separation and enrichment of benzodiazepines in biological samples drugs. The invention belongs to the technical field of separation, enrichment and analysis and detection. 2. Background technology [0002] Benzodiazepines These drugs have sedative, hypnotic, and central skeletal muscle relaxation effects. The clinical manifestations of acute poisoning of the drug are mainly in the muscles and central nervous system, such as muscle weakness, hypotonia, ataxia, dysphonia, lethargy and other symptoms, and severe poisoning manifests as coma, mydriasis, and respira...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/285B01D15/34C08G77/04
Inventor 汤又文金国有
Owner SOUTH CHINA NORMAL UNIVERSITY
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