Core-shell structured stationary phase for chiral ligand exchange chromatography and method for making same

A core-shell structure and chiral ligand technology, applied in the field of analytical chemistry, can solve the problems of low column efficiency, low column capacity and slow mass transfer of stationary phase, and achieve long service life, large column capacity and high selectivity. Effect

Inactive Publication Date: 2006-12-20
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the slow mass transfer in the chromatographic process, the column efficiency of this type of bonded stationary phase is low, and the column capacity is not high, so it is difficult to be used for preparative resolution.

Method used

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  • Core-shell structured stationary phase for chiral ligand exchange chromatography and method for making same
  • Core-shell structured stationary phase for chiral ligand exchange chromatography and method for making same
  • Core-shell structured stationary phase for chiral ligand exchange chromatography and method for making same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) In 150 mL of anhydrous toluene, add 5 mL of vinyltrimethoxysilane and 5 g of silica gel (5 μm, amorphous), react at reflux temperature for 12 h, remove toluene and unreacted vinyltrimethoxysilane by suction filtration , the obtained solid was washed with toluene and methanol in turn, and dried to obtain modified silica gel.

[0020] (2) In 100 mL of anhydrous toluene, add 3 g of modified silica gel, 3 mL of glycidyl acrylate and 60 mg of azobisisobutyronitrile, react at 80°C for 24 hours, filter with suction, and dry the obtained solid by washing with toluene and methanol to obtain Core-shell structured silica gel 1.

[0021] (3) In 100 mL of anhydrous methanol, add 2 g of core-shell structured silica gel 1 and 5 mmol of sodium L-proline, react at 40 °C for 24 h, and filter the obtained solid with methanol, methanol-water (v / v, 5 / 5), washed with water, and dried to obtain CS-LEP I chromatographic stationary phase. Elemental analysis: C 14.88%, H 2.32%, N 0.44%. ...

Embodiment 2

[0024] (1) Prepare modified silica gel according to step (1) of Example 1.

[0025] (2) In 100 mL of anhydrous toluene, add 3 g of modified silica gel, 1 mL of glycidyl acrylate and 20 mg (AIBN), react at 80°C for 2 h, then add 3 mL of glycidyl acrylate and 60 mg of azobisisobutyronitrile, The reaction was continued at 80° C. for 24 hours, and then filtered with suction. The obtained solid was washed with toluene and methanol to obtain silica gel 2 with a core-shell structure.

[0026] (3) The core-shell structure silica gel 2 is used instead of the core-shell structure silica gel 1, and the step (3) of Example 1 is carried out to obtain the CS-LEP II chiral stationary phase of the present invention. Elemental analysis: C 15.28%, H 2.30%, N 0.44%.

[0027] (4) The CS-LEP II stationary phase is used to replace the CS-LEP I phase, and according to the step (4) of Example 1, a chromatographic column and an equilibrium chromatographic column are prepared, and then used for the se...

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Abstract

The invention relates to a chirality ligand exchange spectrum fixing phase of organic-inorganic core frame, and relative preparation, which are used to analyze the chirallity compound, especially for detaching the DL-amino acid and DL-alcoholic acid antimer, wherein on the surface of inorganic particle, grafting polymer macromolecule monomer on the surface, to synthesize the particle with core and frame structure; then using the chirality selection factor chemical decoration, to prepare the fixing phase. The inventive method is simple, with high antimer selectivity, quick detaching speed, and long service life. The accompanying diagram is the detaching spectrum of DL-His (histidine) on fixing phase (CS-LEP I).

Description

technical field [0001] The invention relates to a chiral ligand exchange chromatography stationary phase with an inorganic-organic core-shell structure and a preparation method thereof. The stationary phase is used for high-performance liquid chromatography to resolve chiral compounds, especially DL-amino acids and DLs -Hydroxy acid enantiomer, belonging to the field of analytical chemistry. Background technique [0002] The chromatographic separation of DL-amino acid and DL-hydroxy acid enantiomers on chiral stationary phases can be performed by gas chromatography and liquid chromatography, but usually requires pre-column sample derivatization. The derivatization procedure is time-consuming and troublesome, not only derivatization is required Reagents, and may occur racemization, affecting the analysis results. Chiral ligand exchange chromatography, developed in the 1970s, is an effective method for the separation of chiral compounds, especially amino acids and hydroxy aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/29
Inventor 马言顺龙远德黄天宝
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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