Preparation method and applications of novel imprinting gas chromatography stationary phase

An imprinting and solid technology, which is applied in the field of preparation of nicotine multi-component imprinting composite materials at the same time, can solve the problem of less imprinted polymers, and achieve the effect of high efficiency separation ability and great development potential

Inactive Publication Date: 2020-02-21
JISHOU UNIVERSITY
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AI Technical Summary

Problems solved by technology

Among them, the use of metal-organic framework materials for chromatographic immobilization is a current research hotspot, but

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Preparation of metal-organic framework materials and sulfhydryl modification: In 50mL of deionized water, add 1.0mmol of chromium nitrate nonahydrate and 1.2mmol of terephthalic acid, then add 0.3mL of hydrofluoric acid, and mix the mixture by ultrasonic stirring. Pour it into a 100mL hydrothermal reaction kettle, seal it and react at 493K for 10.5 hours, filter it with suction after cooling, wash the solid with deionized water and N,N-dimethylformamide (DMF) successively, and transfer the solid to Add 50mL of ethanol to the reaction kettle, react at 373K for 18 hours, filter and wash repeatedly with ethanol, vacuum dry, grind and sieve to obtain green solid powder metal organic framework material (A); put 4.0 g metal organic framework material into 250mL Add 100mL of toluene-tetrahydrofuran mixed solvent (volume ratio 1:1) into the flask, stir evenly, add 5.0 mmol of concentrated sulfuric acid and 9.0 mmol of mercaptoacetic acid, and react at 308K for 7 hours. Filt...

Embodiment 2

[0022] (1) Preparation of metal-organic framework materials and sulfhydryl modification: In 50mL of deionized water, add 1.0mmol of chromium nitrate nonahydrate and 2.8mmol of terephthalic acid, then add 0.45mL of hydrofluoric acid, and mix the mixture by ultrasonic stirring. Pour it into a 100mL hydrothermal reaction kettle, seal it and react at 493K for 11 hours, filter it with suction after cooling, wash the solid with deionized water and N,N-dimethylformamide (DMF) successively, and transfer the solid to Add 50mL of ethanol to the reaction kettle, react at 373K for 17 hours, filter and wash repeatedly with ethanol, vacuum dry, grind and sieve to obtain green solid powder metal organic framework material (A); put 4.0 g metal organic framework material into 250mL Add 100mL of toluene-tetrahydrofuran mixed solvent (volume ratio 1:1) into the flask, stir evenly, add 5.0 mmol of concentrated sulfuric acid and 9.0 mmol of mercaptoacetic acid, and react at 308K for 7 hours. Filte...

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Abstract

The invention discloses a nicotine multi-component simultaneous imprinting composite material microsphere preparation method and applications of the microspheres as a gas chromatography stationary phase in separation analysis of difficult-to-separate components in smoke. According to the invention, a composite imprinting material is prepared by using a sulfydryl-modified metal organic framework asa carrier and using a plurality of nicotine mixtures as a common template, a chromatographic column is prepared from the composite imprinting material, and nicotine, nornicotine and neonicotine can be effectively separated under optimized chromatographic conditions, wherein the volume factors of nicotine, nornicotine and neonicotine are respectively 117.8+/-9.01, 83.55+/-4.03 and 71.82+/-5.18; and the obtained material as a gas chromatography stationary phase has selective retention and separation capability on compounds such as nicotine, nornicotine, anabasine and the like in smoke so as toprovide a new method for separation analysis of difficult-to-separate compounds in smoke.

Description

technical field [0001] The invention belongs to the field of new materials, and in particular relates to a preparation method for simultaneously imprinting composite materials of multiple components of nicotine, which is used as a gas chromatography stationary phase to separate and analyze difficult-to-separate compounds in smoke. Background technique [0002] Tobacco is a traditional industry in my country, and it still plays an important role in the development of the national economy. However, "smoking is harmful to health" has restricted the development of the tobacco industry to a certain extent, mainly because tobacco contains a large number of harmful components, which seriously endanger human health, and N-nitrosamines (TSNAs) are one of them . The formation and accumulation of tobacco TSNAs are produced during the tobacco leaf curing process, and are formed by the reaction of nitrogen oxides formed during tobacco pyrolysis with alkaloids such as nicotine and nornic...

Claims

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Application Information

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IPC IPC(8): B01J20/28B01J20/26B01J20/285B01D53/02B01D46/00C08G83/00
CPCB01D46/0036B01D53/02B01D2258/0283B01J20/226B01J20/268B01J20/28021B01J20/285C08G83/008
Inventor 李辉田海希毛琳周丽慧欧美婧曲妍
Owner JISHOU UNIVERSITY
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