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A kind of zwitterion mixed mode chromatography stationary phase and its preparation method and application

A mixed-mode chromatography and zwitterion technology, which is applied to the field of zwitterion mixed-mode chromatography stationary phases and their preparation, can solve the problems of less detection reports and less species, and achieve the effects of precise separation and determination, improving peak shape and reducing environmental pollution.

Active Publication Date: 2022-08-09
INSTITUTE OF ANALYSIS GUANGDONG ACADEMY OF SCIENCES (CHINA NATIONAL ANALYTICAL CENTER GUANGZHOU)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the development of zwitterionic mixed-mode chromatographic stationary phases has been reported, but there are few types; its application is only for the separation of standard solutions, and there are few reports on the detection of samples in different matrices

Method used

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  • A kind of zwitterion mixed mode chromatography stationary phase and its preparation method and application
  • A kind of zwitterion mixed mode chromatography stationary phase and its preparation method and application
  • A kind of zwitterion mixed mode chromatography stationary phase and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0045] The preparation method of the zwitterion mixed mode chromatography stationary phase comprises the following steps:

[0046] (1) Activation of silicon pellets: Weigh 50g silicon pellets into a 500mL three-necked flask, add 300mL hydrochloric acid solution with a mass fraction of 20%, heat and stir to reflux for 24h, cool to room temperature, wash with 100mL distilled water until neutral, It was washed twice with 100 mL of absolute ethanol, and dried in vacuum at 105 °C for 24 h to obtain activated silicon pellets.

[0047] (2) Amino-bonded phase: Weigh 40 g of activated silicon pellets and place them in a 500-mL three-necked flask, add 160 mL of anhydrous toluene and 20 mL of γ-aminopropyltriethoxysilane, stir and reflux for 6 h, cool to room temperature, and sequentially Wash twice with absolute ethanol, water and absolute ethanol, the volume of each washing solution is 100 mL, and vacuum dry at 105° C. for 24 h to obtain an amino-bonded phase. Elemental analysis and c...

Embodiment 2

[0051] Same as Example 1, the difference is:

[0052] Step (3) mercaptoethyl sulfide-based aminopropyl silane bonded phase: weigh 10 g of amino bonded phase into a 250 mL three-neck flask, add 5.0 mL of ethylene sulfide and 100 mL of isopropanol, shake well and sonicate 15min, stirred at room temperature for 2h, then heated to reflux for 6h, cooled to room temperature, washed twice with absolute ethanol, water and absolute ethanol in turn, the volume of each washing solution was 100mL, and vacuum-dried at 105 °C for 24h to obtain sulfhydryl Ethyl polyethyl sulfide aminopropyl silane bonded phase.

[0053] Elemental analysis and characterization results are: C, 6.18%; N, 0.39%; S, 6.95%.

[0054] Step (4) Sulfonic acid ethyl polyethyl sulfone aminopropyl bonded phase: weigh 5 g of mercaptoethyl polyethyl sulfide aminopropyl silane bonded phase into a 125 mL three-neck flask, add 50 mL of peracetic acid, After stirring at room temperature for 24 h, washed with absolute ethanol...

Embodiment 3

[0056] Same as Example 1, the difference is:

[0057] Step (3) Bonded phase of mercaptoethyl polyethyl sulfide aminopropyl silane: Weigh 10 g of amino bonded phase into a 250 mL three-neck flask, add 10.0 mL of ethylene sulfide and 100 mL of isopropanol, shake well and sonicate 15min, stirred at room temperature for 2h, then heated to reflux for 6h, cooled to room temperature, washed twice with absolute ethanol, water and absolute ethanol in turn, the volume of each washing solution was 100mL, and vacuum-dried at 105 °C for 24h to obtain sulfhydryl Ethyl polyethyl sulfide aminopropyl silane bonded phase.

[0058] Step (4) Sulfonic acid ethyl polyethyl sulfone aminopropyl bonded phase: weigh 5 g of mercaptoethyl polyethyl sulfide aminopropyl silane bonded phase into a 125 mL three-neck flask, add 50 mL of peracetic acid, After stirring at room temperature for 24 h, washed with absolute ethanol, water and absolute ethanol for 2 times respectively, the volume of each washing sol...

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Abstract

The invention relates to a zwitterion mixed mode chromatographic stationary phase and a preparation method and application thereof. The stationary phase is based on silicon spheres, and the ligand is composed of sulfonic acid group, amine group and sulfone group. 2 + is an amine cation, SO 3 ‑ is the sulfonic anion, ‑SO 2 ‑ is a sulfone group. The zwitterion mixed mode chromatographic stationary phase proposed by the present invention has a wide application range, and realizes the separation and determination of a total of 23 compounds, such as basic compounds, medium polar compounds and weak polar compounds, under different chromatographic modes.

Description

technical field [0001] The invention belongs to the technical field of liquid chromatography stationary phase materials, in particular to a zwitterion mixed mode chromatography stationary phase and a preparation method and application thereof. Background technique [0002] In the field of contemporary chromatographic analysis, high performance liquid chromatography is one of the most widely used conventional analytical methods, and is now widely used in the fields of food, agricultural products, aquatic products, medicine and chemical industry. With the increase of sample types and the increasingly complex sample matrix, the requirements for chromatographic separation conditions are getting higher and higher, and the choice of chromatographic stationary phase plays a key role in the separation selectivity and separation efficiency of samples. At present, the commercially available chromatographic columns mainly use a single separation mode, with strong separation specificity...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/281B01J20/30G01N30/02
CPCB01J20/286G01N30/02
Inventor 张飞左雄军付强杨熙李镁娟
Owner INSTITUTE OF ANALYSIS GUANGDONG ACADEMY OF SCIENCES (CHINA NATIONAL ANALYTICAL CENTER GUANGZHOU)
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