Solid-phase microextraction coating based on metalloporphyrin microporous polymer, and preparation and application thereof

A technology of microporous polymers and metalloporphyrins, which is applied in the fields of analytical chemistry and environmental analysis, can solve the problems of few separation and analysis applications, and achieve the effects of easy operation and mastery, high thermal stability, and simple production methods

Active Publication Date: 2017-09-05
SUN YAT SEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, CMPs are very effective in gas adsorption, especially for CO 2 It has excellent results in storage, and has reported applications in catalysis, fluorescent sensing, and light harvesting, but it is rarely used in separation analysis, so the application of this type of material in separation analysis remains to be developed

Method used

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  • Solid-phase microextraction coating based on metalloporphyrin microporous polymer, and preparation and application thereof
  • Solid-phase microextraction coating based on metalloporphyrin microporous polymer, and preparation and application thereof
  • Solid-phase microextraction coating based on metalloporphyrin microporous polymer, and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The preparation of the solid-phase microextraction coating based on the metalloporphyrin microporous organic polymer comprises the following steps:

[0046] (1) Preparation of Metalloporphyrin Suspension

[0047] S11: Synthesis of porphyrin-conjugated microporous organic polymers (such as figure 1 shown):

[0048] Tetrabromophenylporphyrin (186.10mg, 0.1mmol), terephthalic acid (33.15mg, 0.2mmol), and 8ml of 1,4-dioxane were added to the flask, mixed evenly by ultrasonication, frozen-pump- Thaw cycle three times to remove oxygen and add K 2 CO 3 Solution 2.0ml (110.4mg, 0.8mmol) and catalyst Pd (PPh 3 ) 4 (11.6mg, 10μmol), put it in a microwave oven, freeze-pump-thaw cycle three times, the stirring speed is 800rpm, under the protection of nitrogen, under the optimal conditions, select the microwave power of 100w, the reaction temperature is 90℃, the reaction time is 90min, the reaction is over Afterwards, the reaction solution was filtered with suction, and the p...

Embodiment 2

[0059] Identification of Volatile Aroma Substances in Chinese Zanthoxylum bungeanum in Example 2

[0060] (1) Sample processing method: Grind the Zanthoxylum bungeanum sample, sieve it, weigh 200 mg of the sample in 20 ml of solid-phase microextraction headspace product, equilibrate in a water bath at 60 ° C for 30 minutes, and mix the solid-phase microextraction prepared in Example 1 Insert the head into the headspace bottle, extract for 30min, and finally keep the quartz fiber in the gas chromatography inlet for 3min. Figure 4 It is a schematic diagram of solid phase microextraction coating preparation and extraction process.

[0061] (2) Gas chromatography conditions for Zanthoxylum bungeanum: carrier gas: He gas, column flow rate, 1mL / min; sampling method: split flow; split ratio: 5:1; chromatographic column: Agilent DB-5MS (30m×0.25mm×0.25μm) ;Injection port temperature: 200°C; temperature program: 60°C without holding, 2°C / min up to 85°C without hold, 8°C / min up to 200...

Embodiment 3

[0065] Identification of volatile aroma substances in the bay leaf of embodiment 3

[0066] (1) Sample processing method: Grind and sieve the bay leaf sample, weigh 200 mg of the sample into 20 ml of solid-phase microextraction headspace product, equilibrate in a 60°C water bath for 30 minutes, and mix the solid-phase microextraction prepared in Example 1 Insert the extraction head into the headspace bottle, extract for 30 minutes, and finally keep the fiber in the gas chromatography inlet for 3 minutes.

[0067] (2) Germ leaf gas chromatography conditions: carrier gas: He; column flow rate, 1mL / min; sample injection method: split flow; split ratio: 5:1; chromatographic column: Agilent DB-5MS (30m×0.25mm×0.25μm) ;Injection port temperature: 200°C; Temperature program: 60°C not maintained, 2°C / min to 90°C, 5°C / min to 200°C, 10°C / min to 220°C and hold for 2min; Transfer line temperature, 250 ℃.

[0068] Mass spectrometry conditions: quadrupole; scanning method: SCAN; scanning ...

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Abstract

The invention relates to a solid-phase microextraction coating based on a metalloporphyrin microporous polymer, and a preparation method and an application thereof. The preparation method for the solid-phase microextraction coating based on the metalloporphyrin microporous polymer comprises the following steps: preparing a metalloporphyrin suspension, pretreating solid-phase microextraction fiber, and coating the metalloporphyrin suspension on the surface of the solid-phase microextraction fiber so as to obtain the solid-phase microextraction coating based on the metalloporphyrin microporous polymer, wherein the metalloporphyrin suspension is prepared through the following steps: S11: preparation of a porphyrin conjugated microporous organic polymer under the condition of microwave synthesis; S12: synthesis of a metalloporphyrin conjugated microporous organic polymer through an action of the porphyrin conjugated microporous organic polymer and metal salt; and S13: preparation of the metalloporphyrin suspension from the metalloporphyrin conjugated microporous organic polymer. The coating prepared by using the method provided by the invention has the advantages of good thermal stability, strong enrichment capacity, etc., can be applied to extraction heads for solid-phase microextraction, and has an effective application in the fields of food analysis, environment analysis, etc.

Description

technical field [0001] The invention relates to the fields of analytical chemistry and environmental analysis, in particular to a solid-phase microextraction coating based on a metalloporphyrin microporous polymer and a preparation method and application thereof. Background technique [0002] Solid-phase microextraction (solid-phase microextraction, SPME) technology was proposed by Pawlinszyn of University of Waterloo, Canada and his collaborator Arthur in 1989. Solid-phase microextraction overcomes the defects of traditional sample pretreatment technology, integrating sampling, extraction, Concentration and sample injection are integrated, which reduces the tedious sample processing process and reduces the analysis and detection time. Its remarkable technical advantages are being widely concerned by analysts in the environment, food, and pharmaceutical industries, and are being vigorously promoted. In solid phase microextraction One of the limiting factors in the developmen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/28B01J20/281B01J20/30B01J20/32C08G61/12G01N30/02
CPCG01N30/02C08G61/124B01J20/28023B01J20/281B01J20/3204B01J20/3272B01J20/3291C08G2261/344C08G2261/411C08G2261/592C08G2261/962C08G2261/18C08G2261/3241
Inventor 胡玉玲李攻科彭毅
Owner SUN YAT SEN UNIV
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