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Iminazole type ionic liquid reversed phase electrochromatography organic monolithic column

An ionic liquid, imidazole type technology, applied in the field of analytical chemistry, to achieve the effect of good shape, low rigidity improvement and irreversible tailing phenomenon

Active Publication Date: 2013-05-08
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention adopts the green solvent ionic liquid as a new type of ionic compound monomer, which can dissolve the long carbon chain neutral monomer very well, and solves the problem of mutual solubility between the ionic compound monomer and the neutral monomer

Method used

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  • Iminazole type ionic liquid reversed phase electrochromatography organic monolithic column
  • Iminazole type ionic liquid reversed phase electrochromatography organic monolithic column
  • Iminazole type ionic liquid reversed phase electrochromatography organic monolithic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] （1） Pretreatment of the column

[0022] The quartz capillary empty column is first flushed with 0.1 mol / L NaOH for 2 h to 3 h, then with deionized water for 10 min, then with 0.1 mol / L HCl solution for about 1 h, and then with methanol for 30 min. Blow dry and set aside.

[0023] （2） This step is optional.

[0024] Add a 1:1 mixture of methanol and methacryloxypropyltrimethoxysilane to the capillary treated in step 1, and react at 60°C for 12 to 24 h. Then rinse with methanol for 20 min to 30 min. Blow dry with nitrogen at 70°C.

[0025] (3) In-column synthesis

[0026] Lauryl methacrylate (functional monomer), ethylene dimethacrylate (crosslinking agent), 1-allyl-3-methylimidazole hexafluorophosphate, porogen and initiator Prepared according to the following mass percentage data:

[0027] Column A: Neutral compound 25%, methanol: 2.5%, n-propanol: 25%, 1,4-butanediol: 36.5%, initiator azobisisobutyronitrile 1%.

[0028] Column B: Neutral compound 24.75%, 1-allyl-3-methylimidaz...

Embodiment 2

[0037] In order to verify the separation performance of the developed imidazole-type ionic liquid reversed-phase electrochromatographic organic monolithic column for neutral homologues, the monolithic column D prepared above was used with acetonitrile: phosphate buffer salt (5 mmol / L, pH=7.0) = 70:30 is the mobile phase, the separation voltage is +10 kV, the auxiliary pressure is 1.2 MPa, and the pump flow rate is 0.1 ml / min. Neutral benzene series are baseline separated on the positively charged hydrophobic interaction organic monolithic column. The elution peaks are: 1 thiourea, 2 toluene, 3 ethylbenzene, 4 propylbenzene, 5 butylbenzene, 6 pentylbenzene.

Embodiment 3

[0039] In order to verify the separation performance of the developed imidazole-type ionic liquid reversed-phase electrochromatographic organic monolithic column for polycyclic aromatic hydrocarbons, the monolithic column D prepared above was used with acetonitrile: phosphate buffer salt (5 mmol / L, pH=7.0)=80 : 20 is the mobile phase, the separation voltage is +15 kV, the auxiliary pressure is 1.2 MPa, and the pump flow rate is 0.1 ml / min. Polycyclic aromatic hydrocarbons achieve baseline separation on the reversed-phase electrochromatographic organic monolithic column and the elution peak The order is: 1 thiourea, 2 naphthalene, 3 phenanthrene, 4 anthracene.

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Abstract

The invention discloses an iminazole type ionic liquid reversed phase electrochromatography organic monolithic column. A monolithic stationary phase is a porous continuous bed formed by in situ polymerization of neutral compound and ionic compound monomer; the neutral compound is methacrylic acid dodecyl ester and dimethyl crylic acid ethyl diester, the ionic compound monomer is 1-allyl-3-methylimidazole phosphate ionic liquid, the pore-forming agent is one or more of methyl alcohol, methylbenzene, normal propyl alcohol, cyclohexanol, capryl alcohol, 1,4-butanediol and ethylene glycol, and the initiator is azodiisobutyronitrile. The iminazole type ionic liquid reversed phase electrochromatography organic monolithic column provided by the invention not only has typical reversed phase chromatographic performance, but also can provide ion exchange groups and generate higher electroosmotic flow, change polymerization quantity of ionic liquid and change the size of the electroosmotic flow. The stationary phase of the monolithic column can meet the requirement on rapid separation of polar compound, neutral compound and alkali compound.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to an organic monolithic column of imidazole-type ionic liquid reversed-phase electrochromatography. Background technique [0002] Capillary electrochromatography (CEC) is a micro-separation technique that combines the high selectivity of high performance liquid chromatography (HPLC) and the high efficiency of capillary electrophoresis (CE). The mobile phase is driven by electroosmotic flow or electroosmotic flow and pressure flow, so its separation process has the characteristics of multi-mechanism synergy. [0003] As an important stationary phase for CEC separation, capillary monolithic column has the advantages of simple preparation, good permeability, no need for plunger and easy modification, etc. It has become a research hotspot in the field of modern micro-separation. At present, monolithic chromatographic columns are mainly divided into two categories: organ...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01D15/22B01D15/08B01J20/285B01J20/30C08F220/18C08F222/14C08F226/06C08J9/28
Inventor 吴晓苹吴祥宗蔡晓蓉
Owner FUZHOU UNIV
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