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Formula of raw material of reversed phase ion exchange electrochromatography column, and preparation method

A reverse-phase ion and electrochromatographic column technology, applied in the field of electrochromatography, can solve problems such as inability to dissolve, large polarity difference, and research limitations, and achieve the effects of good column permeability and a wide range of pH applications

Inactive Publication Date: 2010-11-17
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the monolithic columns studied now contain short alkyl chains (isopropyl, butyl, hexyl, dodecyl) (A.Palm, M V Novotny, Anal.Chem.69 (1997) 4499), while To make monolithic columns with long alkyl chains (C17, C18, C20), due to the large difference in polarity between neutral monomers and ionic compound monomers, even the best porogens cannot dissolve them, so their Research is restricted

Method used

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  • Formula of raw material of reversed phase ion exchange electrochromatography column, and preparation method
  • Formula of raw material of reversed phase ion exchange electrochromatography column, and preparation method
  • Formula of raw material of reversed phase ion exchange electrochromatography column, and preparation method

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preparation example Construction

[0015] The steps of preparation method are:

[0016] 1) Pretreatment of the column: Rinse the empty capillary column with 0.1-1mol / l HCl solution for about 15-30min, then rinse with deionized water for 10-15min, then rinse with 0.1-1mol / l NaOH for 2h-3h, then Rinse with methanol for 15-20 minutes, blow dry with nitrogen and set aside.

[0017] 2) This step is optional: add a 1-2:1 mixture of methanol and methacryloxypropyltrimethoxysilane to the treated capillary in step 1), and react at 40-60°C for 12h-24h. Then rinse with methanol for 10min to 15min. Blow dry with nitrogen at 50-70°C.

[0018] 3) In-column synthesis: mix the raw materials according to the above formula, ultrasonically vibrate the resulting mixture for 10-15 minutes, blow nitrogen to remove the dissolved oxygen in the mixture, then inject the mixture into the treated capillary, seal both ends of the capillary and Immerse in a 60°C water bath and react for 5-20 hours. After the reaction is completed, wash t...

Embodiment 1

[0020] 1. Column pretreatment

[0021] First rinse the capillary empty column with 0.1mol / l HCl solution for about 0.5h, then rinse it with deionized water for 10min, then rinse it with 0.1mol / l NaOH for 2h~3h, then rinse it with methanol for 15min, and dry it with nitrogen gas for later use.

[0022] 2. This step is optional. Add a 1:1 mixture of methanol and methacryloxypropyltrimethoxysilane to the capillary treated in step 1, and react at 60°C for 12h to 24h. Then rinse with methanol for 10min to 15min. Blow dry at 70°C with nitrogen.

[0023] 3. In-column synthesis

[0024] Octadecyl methacrylate, ethylene glycol dimethacrylate, 3-propanesulfonic acid methacrylate, cyclohexanol and 1,4-butanediol are respectively 17.82% by weight: 12.00%: 0.18 %: 49.00%: 21.00%, the consumption of the added initiator azobisisobutyronitrile (AIBN) is 1% of the polymer monomer consumption, after the mixture is ultrasonically vibrated for 20min, blow nitrogen for 10min to remove dissolve...

Embodiment 2

[0026] Octadecyl methacrylate, ethylene glycol dimethacrylate, 2-methylpropionyl ethyltrimethylammonium ethyl sulfate, cyclohexanol and 1,4-butanediol are respectively by weight 17.70%: 12.00%: 0.30%: 45.50%: 24.50%, the amount of the added initiator azobisisobutyronitrile is 1% of the amount of the polymer monomer, after the mixture is ultrasonically oscillated for 20 minutes, nitrogen gas is blown for 10 minutes to remove the dissolved oxygen, inject the reaction solution into a capillary of a certain length that has been treated according to step 2, seal both ends of the capillary, and immerse in a water bath at 60°C, and react for 10 hours. After the reaction is completed, first use methanol and then use Rinse the mobile phase to remove the reagents that may remain in the capillary. Finally, the column is equilibrated for 15 hours in a low voltage state to perform normal experiments or save for future use.

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Abstract

The invention provides a raw material formula of the anti-phase ion exchange electricity chromatographic column: ionic compound monomer; neutral compound monomer; initiator; the hole-making. According to the above raw material formula, the neutral compound monomer and the ionic compound monomer carries on the polyreaction in the capillary vessel, joins the hole-making and the initiator in the polyreaction, then prepares the anti-pjase ion exchange electricity chromatographic column. The invention has solved the mutual solubility question which between the ionic compound monomer and the neutral monomer, may satisfies the continuously sharp separation request of the neutrality, acidity and alkaline matter; the pillar has good insightful performance, is suitable to the high concentrated buffer salt system; when preparing, no longer need to burn the plug on the two ends of the pillar, also has avoided the difficulty of filling up the pillar.

Description

technical field [0001] The invention relates to electrochromatography technology, more specifically to a raw material formula of a reversed-phase ion-exchange electrochromatographic column and a preparation method thereof. Background technique [0002] Capillary electrochromatography (CEC) is a micro-separation technology combining high performance liquid chromatography (HPLC) and capillary electrophoresis (CE). Its mobile phase is driven by electroosmotic flow in the tube. Efficiency of electrophoresis. There are currently three types of electrochromatographic columns: capillary packed columns, capillary open-tube columns, and capillary monolithic columns. Packed columns have been developed rapidly recently, but the plunger must be prepared, and the stopper usually causes the generation of air bubbles, which may cause the interruption of the experimental run. Although the open-tube column has no sealing problem and can obtain higher column efficiency, it is also limited b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/287
Inventor 谢增鸿林坚林旭聪吴晓苹
Owner FUZHOU UNIV
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