Polymer monolithic column, solid phase extraction filter based on same, and preparation method and application thereof

A polymer and monolithic column technology, applied in the field of chemical separation, can solve the problems of poor extraction effect of polar and strongly polar compounds, silica gel matrix can not be used in alkaline environment, can not meet the actual sample analysis requirements, etc., to achieve specification selection The effect of wide range, cheap raw materials, and simplified cost

Active Publication Date: 2017-07-14
INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the C8 / C18 solid-phase extraction column has the following limitations: (1) This type of extraction column is hydrophobic and is only suitable for adsorption of strong non-polar, non-polar and neutral compounds, and for polar and strongly polar compounds The extraction effect is not good; (2) before use, it must be activated with an organic solvent such as methanol, so that the alkyl chain on the surface of this type of column is in an extended state, so that it can better contact the target compound, but the activation step is often complicated and time-consuming. (3) The silica gel matrix cannot be used in an alkaline environment, which limits the scope of application of this type of solid-phase extraction column
However, monolithic solid-phase extraction columns still have limitations such as single type, poor repeatability, small adsorption capacity, complex and time-consuming operation, and are far from meeting the analysis needs of actual samples.

Method used

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  • Polymer monolithic column, solid phase extraction filter based on same, and preparation method and application thereof
  • Polymer monolithic column, solid phase extraction filter based on same, and preparation method and application thereof
  • Polymer monolithic column, solid phase extraction filter based on same, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0108] Embodiment 1 Preparation of solid phase extraction syringe filter based on monolithic column

[0109] Weigh 10.0mg of azobisisobutyronitrile, 300mg of methacryloylethylsulfobetaine, 300mg of methylenebisacrylamide, 1.25mL of dimethyl sulfoxide, 1.25mL of methanol and 1.00mL of n-dodecyl alcohol, and sonicate for 20min Make it evenly mixed, inject the above polymerization liquid into a needle filter (13mm i.d.) through a syringe, then seal both ends of the needle filter with raw material tape, parafilm, and scotch tape in turn, and put it in a water bath at 80°C for standing 12h. After the polymerization reaction is completed (the schematic diagram of the polymerization reaction is as follows figure 1 shown), connect the syringe filter to the syringe (eg figure 2 ), inject a certain amount of methanol from the end of the syringe, push the methanol out, and make it flow through the needle filter of the solid phase extraction based on the monolithic column to remove the...

Embodiment 2

[0110] Example 2 Extraction and separation of steroid drugs using solid phase extraction filters based on monolithic columns

[0111] Utilize the solid-phase extraction syringe filter based on the monolithic column described in Example 1 to enrich the trace steroid drugs in the aqueous phase: add 10 mL of the aqueous solution of seven trace steroid drugs (0.550 μg / mL progesterone, 0.555 μg / mL testosterone, 0.603 μg / mL megestrol acetate, 0.590 μg / mL cyproterone acetate, 0.617 μg / mL levonorgestrel, 0.583 μg / mL progesterone caproate, 0.574 μg / mL testosterone propionate), release this solution, and after the solution all flows out, release 1 mL of deionized water to clean the remaining impurities on the monolithic column, and then release 1 mL of methanol to obtain the eluent. Finally, the collected eluate was analyzed by high performance liquid chromatography.

[0112] Chromatographic conditions: Chromatographic column: XD6-C18 (5μm, 150mm x 4.6mm i.d., Agilent); mobile phase: m...

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Abstract

The invention belongs to the technical field of chemical separation and particularly relates to a polymer monolithic column, a solid phase extraction filter based on same, and a preparation method and an application thereof. The polymer is prepared through an in-situ polymerization reaction of a monomer, a crosslinker, a pore former and an initiator. The monolithic column and the solid phase extraction filter can perform selective extraction to a to-be-tested target substance or impurity according to demands on separated samples. Compared with a conventional hydrophobic solid phase extraction material, the monolithic column and the solid phase extraction filter have a wider coverage of applicable objects. Compared with a conventional packed solid phase extraction small column, the monolithic column can give consideration to both separation speed and recovery ratio, so that the extraction and separation efficiency is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of chemical separation, and in particular relates to a polymer monolithic column, a solid phase extraction filter based on the monolithic column, a preparation method and application thereof. Background technique [0002] Sample pretreatment is an indispensable step in analytical chemistry methods and is crucial to improving the precision and accuracy of sample analysis. In recent years, as the types of organic compounds continue to increase and the matrices become increasingly complex and diverse, sample pretreatment techniques are facing new challenges. Solid phase extraction technology is one of the most effective sample pretreatment technologies. It has both extraction and concentration functions, and has the advantages of less consumption of organic solvents and high extraction efficiency. It is widely used in medicine, food science, environmental science and other fields. Sample pretreatment in progre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/38C08F220/38C08J9/28B01J20/285B01D15/22B01J20/30
CPCB01D15/22B01J20/285C08F220/38C08F222/385C08J9/28C08J2333/14C08J2435/00C08F220/387
Inventor 李楠邱静钱永忠宋月
Owner INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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