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A kind of organotin molecularly imprinted polymer microsphere, solid phase extraction column and application thereof

A technology of molecular imprinting and polymers, which is applied in the fields of alkali metal compounds, inorganic chemistry, separation methods, etc., can solve the problems of non-compliance, increased extraction times and costs, and molecular imprinted polymers have not yet been seen, achieving low usage and excellent quality Adsorption performance, cost reduction effect

Active Publication Date: 2018-05-11
BEIJING PURKINJE GENERAL INSTR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the application of molecularly imprinted materials in sample pretreatment is limited to a single target, and most of them need to prepare several molecularly imprinted polymers in batches to enrich multiple targets, which increases the number of extractions and costs, which is not in line with the current multi- Requirements for Residue Detection Technology
Up to now, there has not been a single report of molecularly imprinted polymers enriched with multiple organotins at the same time

Method used

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  • A kind of organotin molecularly imprinted polymer microsphere, solid phase extraction column and application thereof
  • A kind of organotin molecularly imprinted polymer microsphere, solid phase extraction column and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] This example provides a preparation method of organotin molecularly imprinted polymer microspheres, and its application as a MISPE column prepared as a filler.

[0062] A) Dissolve the double template molecules of dibutyltin chloride (DBT) and diphenyltin chloride (DPT) and 0.14mL methacrylic acid (MAA) in 2mL of dichloromethane, then add a certain amount of acetonitrile , pre-action in the oscillator for 25 minutes;

[0063] Wherein, the final concentrations of DBT and DPT in the final inert solvent system are each 0.1mmol; the final concentration of the methacrylic acid is 0.7mmol;

[0064] B) Add 0.1825mL TRIM (final concentration 0.6mmol) and 40.0mg AIBN to the mixture in A) and mix thoroughly. Ultrasound at room temperature for 5 minutes, nitrogen deoxygenation for 10 minutes, and then seal;

[0065] C), heating in a constant temperature water bath at 55°C for 26 hours, cooling, centrifuging, sieving, discarding the supernatant to obtain a precipitate, and then d...

Embodiment 2

[0070] This example provides a preparation method of organotin molecularly imprinted polymer microspheres, and its application as a MISPE column prepared as a filler.

[0071] A) Dissolve the dual template molecules of dibutyltin chloride (DBT) and diphenyltin chloride (DPT) and 0.3mL methacrylic acid (MAA) in 2mL of dichloromethane, then add a certain amount of acetonitrile , pre-action in the oscillator for 35 minutes;

[0072] Wherein, the final concentrations of DBT and DPT in the final inert solvent system are each 0.3mmol; the final concentration of the methacrylic acid is 1.5mmol;

[0073] B) Add 0.5475mL TRIM (final concentration 1.8mmol) and 40.0mg AIBN to the mixture in A) and mix thoroughly. Ultrasound at room temperature for 5 minutes, nitrogen deoxygenation for 10 minutes, and then seal;

[0074] C), heating in a constant temperature water bath at 65°C for 22 hours, cooling, centrifuging, sieving, discarding the supernatant to obtain a precipitate, and then dryi...

Embodiment 3

[0079] This example provides a preparation method of organotin molecularly imprinted polymer microspheres, and its application as a MISPE column prepared as a filler.

[0080] A), dissolve the double template molecules of dibutyltin chloride (DBT) and diphenyltin chloride (DPT) and 0.24mL methacrylic acid (MAA) in 2mL of dichloromethane, then add a certain amount of acetonitrile , pre-action in the oscillator for 30 minutes;

[0081] Wherein, the final concentrations of DBT and DPT in the final inert solvent system are each 0.2mmol; the final concentration of the methacrylic acid is 1.2mmol;

[0082] B) Add 0.365mL TRIM (final concentration 1.2mmol) and 40.0mg AIBN to the mixture in A) and mix thoroughly. Ultrasound at room temperature for 5 minutes, nitrogen deoxygenation for 10 minutes, and then seal;

[0083] C), heating in a constant temperature water bath at 60°C for 24 hours, cooling, centrifuging, sieving, discarding the supernatant to obtain a precipitate, and then d...

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Abstract

The invention relates to the field of compound extraction and separation purification and especially relates to an organotin molecularly imprinted polymer microsphere, a solid phase extraction column filled with the organotin molecularly imprinted polymer microspheres and a use of the solid phase extraction column. Dibutyltin chloride and diphenyltin chloride as template molecules, methacrylic acid as a functional monomer, trimethylolpropane trimethacrylate as a crosslinking agent and azodiisobutyronitrile as an initiator undergo a reaction in an inert solvent and then the template molecules in the reaction product are removed so that the molecularly imprinted polymer is obtained. The solid phase extraction column realizes specific separation and enrichment of six organotin compounds.

Description

technical field [0001] The invention relates to the field of compound extraction and separation and purification, in particular to an organotin molecularly imprinted polymer microsphere, a solid phase extraction column and applications thereof. Background technique [0002] Organotin is a kind of metal-organic compound containing tin, which is widely used in many fields such as industry, agriculture, textile industry and shipbuilding industry. It is mainly used as PVC stabilizer, wood preservative, antifouling paint, agricultural insecticide, textile Preservatives, etc., because these substances are highly toxic to organisms under the enrichment of the food chain, and can cause endocrine disorders and neurological diseases. The Joint Expert Committee on Environmental Hormones with the Organization for Development (OECD) identified endocrine disruptors (EEDs) with androgen-like effects. As one of the important persistent toxic substances (PTS), the pollution of organotin com...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/06C08F222/14C08F2/02C08J9/26B01J20/26B01J20/28B01J20/30B01D15/20G01N30/60
CPCB01D15/20B01J20/268B01J20/28021C08F2/02C08F220/06C08J9/26C08J2333/02G01N30/6052C08F222/103
Inventor 佘永新王静张超赵风年王珊珊金茂俊金芬邵华郑露飞
Owner BEIJING PURKINJE GENERAL INSTR
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