Broad-spectrum solid phase extracting filler and its application

A broad-spectrum, extraction technology, applied in the field of broad-spectrum solid phase extraction packing, can solve the problems of increased experimental intensity and cost, huge differences in properties, and a single adsorbent covers multiple types of compounds, achieving low price, simple preparation method, good quality and so on. The effect of adsorption performance

Inactive Publication Date: 2017-02-22
JINAN UNIVERSITY +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the wide variety of commonly used pesticides and the huge difference in properties between the compounds, it is difficult to use a single adsorbent to cover multiple types of compounds from polar to non-polar. Therefore, the detection of different types of pesticides and Metabolites, often need to choose different types of SPE column fillers in batches, resulting in increased experiment intensity and cost

Method used

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  • Broad-spectrum solid phase extracting filler and its application
  • Broad-spectrum solid phase extracting filler and its application
  • Broad-spectrum solid phase extracting filler and its application

Examples

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preparation example Construction

[0027] A broad-spectrum solid-phase extraction filler, its synthesis method comprises the following steps: 1-vinylimidazole, divinylbenzene, azobisisobutyronitrile and acetonitrile are mixed, after ultrasonic treatment, remove oxygen under airtight condition at 50 React at ~70°C for 6-36 hours; pulverize and sieve the obtained product, sieve the product with a particle size of 40-60 μm, clean it, and dry it to obtain a broad-spectrum solid-phase extraction filler.

[0028] Preferably, the molar ratio of 1-vinylimidazole to divinylbenzene is 1:5˜5:1.

[0029] Preferably, the amount of azobisisobutyronitrile used is 1%-3% of the sum of the mass of 1-vinylimidazole and divinylbenzene.

[0030] Preferably, the molar volume ratio of 1-vinylimidazole to acetonitrile is (2-10) mmol: (5-15) mL.

[0031] Preferably, the ultrasonic treatment time is 15-30 minutes.

[0032] Preferably, the method for removing oxygen is filling with nitrogen or inert gas.

[0033] Preferably, the produ...

Embodiment 1

[0051] The synthetic method of embodiment 1 broad-spectrum solid-phase extraction filler

[0052] Dissolve 10 mmol of 1-vinylimidazole and 2 mmol of divinylbenzene in 5 mL of acetonitrile solution, add 30 mg of azobisisobutyronitrile, ultrasonically disperse for 20 min, fill with nitrogen and deoxygenate for 10 min, and seal. React under water conditions of 60°C for 24 hours to obtain a lumpy product, then grind the product, sieve, and sieve the product with a particle size of 40-60 μm. Then, the sieved polymer was ultrasonically cleaned with methanol solution for 5 times, each time for 30 minutes, to remove excess reactants, and dried at 60°C for 24 hours to obtain a broad-spectrum solid-phase extraction filler for future use.

[0053] The broad-spectrum solid-phase extraction filler that this embodiment prepares is figure 1 White powdery granules shown.

[0054] figure 2 Be the BET test isothermal adsorption-desorption curve of the broad-spectrum solid-phase extraction f...

Embodiment 2

[0057] The synthetic method of embodiment 2 broad-spectrum solid-phase extraction filler

[0058] Dissolve 10 mmol of 1-vinylimidazole and 2 mmol of divinylbenzene in 15 mL of acetonitrile solution, add 12 mg of azobisisobutyronitrile, ultrasonically disperse for 15 min, fill with nitrogen and deoxygenate for 10 min, and seal. React for 36 hours at 50°C in water to obtain a lumpy product, then grind the product, sieve, and sieve the product with a particle size of 40-60 μm. Then, the sieved polymer was ultrasonically cleaned with methanol solution for 6 times, 20 minutes each time, to remove excess reactants, and dried at 55°C for 20 hours to obtain a broad-spectrum solid-phase extraction filler for future use.

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Abstract

The invention discloses a broad-spectrum solid phase extracting filler and its application. The filler is prepared by mixing 1-vinyl imidazole, divinyl benzene, azodiisobutyronitrile and acetonitrile, and reacting at 50-70 DEG C; crushing, screening, cleaning and drying the product obtained. The specific area of the filler is 300-365 m2 / g, the pore volume and mean pore size are 0.092 cm3 / g and 2.22 nm respectively; the filler is applicable to analyze many kinds of insecticides and metabolites with wide polar scale at the same time, and has relatively high recycle rate and precision for 48 insecticides and metabolites from high polarity to non-polarity in a water body, including anabasine, phenyl pyrazol, organophosphorus, organic chloride, and pyrethroids.

Description

technical field [0001] The invention relates to a broad-spectrum solid-phase extraction filler and its application. Background technique [0002] With the continuous increase in the use of pesticides, their pollution problems are common, and many types of pesticides and metabolites are frequently detected in various environmental media. Pesticides and metabolites in environmental water generally need to undergo pretreatment steps such as enrichment and purification before instrumental detection. Commonly used enrichment and purification methods include liquid-liquid extraction (LLE), solid-phase extraction ( Solid phase extraction (SPE), solid phase microextraction (solid phase microextraction, SPME), single droplet microextraction (suspended droplet microextraction, SDME), stir bar adsorption extraction (stir bar sorptive extraction, SBSE) and other methods. Among them, the SPE method is the most common. However, due to the wide variety of commonly used pesticides and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F226/06C08F212/36G01N30/02G01N30/06B01J20/26B01J20/281B01J20/30
CPCB01J20/261B01J20/281C08F212/36C08F226/06G01N30/02G01N30/06
Inventor 熊晶晶李慧珍游静
Owner JINAN UNIVERSITY
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