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Novel hydrophilic C18 filling material and its solid phase extraction column

A solid-phase extraction column and a new technology, applied in the field of analytical chemistry, can solve the problems of poor recovery rate of strongly water-soluble samples, and achieve the effects of good adsorption effect, easy mass production, and wide application range.

Inactive Publication Date: 2012-02-15
天津博纳艾杰尔科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, the above materials all have their defects, especially the silica gel material has a poor recovery rate for strongly water-soluble samples. Therefore, it is necessary to develop a C18 filler that has a strong binding ability with water, can extract strongly water-soluble samples from water, and enhance gas Recovery rate

Method used

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  • Novel hydrophilic C18 filling material and its solid phase extraction column
  • Novel hydrophilic C18 filling material and its solid phase extraction column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of Two New Materials of Functional Group Bonded Silica Gel

[0029] Add 5000ml of toluene to a 10000ml four-neck flask with a pore size of 1.5kg Silica gel, dehydrated to anhydrous state (1min anhydrous drop shall prevail), then lower the temperature to 80°C, add pre-mixed silane (octadecyltrichlorosilane:methyltrimethoxysilane=8:2; note: mix The ratio is mass ratio) 600g, then add 400g of imidazole, raise the temperature to 120°C, keep the temperature at 120±1°C for 12 hours, then cool and discharge.

[0030] Dry the above filler with a centrifuge, wash it three times with 4500ml of toluene, wash it three times with 4500ml methanol, soak it in a mixed solution of 4000ml tetrahydrofuran and 300ml water for one hour, then wash it three times with 4500ml tetrahydrofuran, and wash it three times with 4500ml methanol , and then dried under vacuum at 100°C for 10 hours to obtain the finished product.

Embodiment 2

[0032] Preparation of step-by-step bonding of two new silica gel materials with functional groups

[0033] Step 1: Add 5000ml of toluene and 1.5kg of pore size to a 10000ml four-neck flask Silica gel, dehydrated to anhydrous state (1min no water drops shall prevail), then cooled to 80°C, added 500g of octadecyltrimethylchlorosilane, then added 300g of imidazole, heated to 120°C, and 120±1°C Keep warm for 12 hours, cool and discharge.

[0034] Dry the above filler with a centrifuge, wash it three times with 4500ml of toluene, wash it three times with 4500ml methanol, soak it in a mixed solution of 4000ml tetrahydrofuran and 300ml water for one hour, then wash it three times with 4500ml tetrahydrofuran, and wash it three times with 4500ml methanol , and then dried under vacuum at 100°C for 10 hours to obtain a semi-finished product.

[0035] The second step: Add 5000ml of toluene and the semi-finished product obtained from the above reaction into a 10000ml four-neck flask, de...

Embodiment 3

[0038] Weigh 500mg of the new material for surface modification of silica gel, put it into a 6ml column tube with a lower sieve plate, fill it into the upper sieve plate, vibrate evenly with a vibrating bed, and compact it with a column press.

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Abstract

The invention relates to a resin surface modified novel material and a solid phase extraction column, which relates to the chemical technical field. The solid phase extracting resin surface modified novel material has the difference of the mean particle diameter in a range of between -20 and 20 percent, the difference of the specific weight is in a range of between -20 and 20 percent. The solid phase extraction mixed filling material is used for preparing the solid phase column, the mixed filling material is filled in the column tube, sieve plates are provided outside of two ends of the filling material for preventing the mixed filling material from leaking, one end of the column tube is for loading and the other end of the column tube is for flowing out, an eluent enters into the solid phase extraction column from a loading aperture. The characteristic application of the present invention is a selective extraction of a polar and nonpolar compound in a solution under water environment.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to a new material with two functional groups bonded on the surface of silica gel and a solid-phase extraction column thereof. Background technique [0002] The new hydrophilic C18 material is a widely used filler for sample pretreatment technology. The basic principle of sample pretreatment technology is solid phase extraction. The components in the sample that have a strong interaction with the stationary phase are retained on the solid phase extraction column. The components with weaker force with the stationary phase flow out of the solid phase extraction column quickly, so as to achieve the purpose of separation. [0003] Currently, the most widely used solid phase extraction materials are mainly bonded silica solid phase extraction materials, inorganic matrix solid phase extraction materials, organic polymer solid phase extraction materials and mixed solid phase ex...

Claims

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Application Information

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IPC IPC(8): B01J20/286B01D15/08
Inventor 李海涛
Owner 天津博纳艾杰尔科技有限公司
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