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MOF@SiO2 core-shell microsphere HPLC chiral column for enantiomeric resolution

A technology of enantiomers and chiral columns, applied in the field of chiral separation of high performance liquid chromatography, can solve the problems of low column efficiency of chiral MOFs columns, difficulty in obtaining stationary phase particles, and affecting the separation performance of chromatographic columns. Achieve excellent separation performance, low cost of column production, and simple method

Active Publication Date: 2019-04-19
YUNNAN NORMAL UNIV
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  • Summary
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the irregular shape and wide size distribution of most of the synthesized MOFs particles, it is difficult to obtain ideal stationary phase particles even by grinding and solvent flotation, which makes the column efficiency of the prepared chiral MOFs column low and the background High pressure, which affects the separation performance of the column

Method used

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  • MOF@SiO2 core-shell microsphere HPLC chiral column for enantiomeric resolution
  • MOF@SiO2 core-shell microsphere HPLC chiral column for enantiomeric resolution
  • MOF@SiO2 core-shell microsphere HPLC chiral column for enantiomeric resolution

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Effect test

Embodiment 1

[0021] 1. Preparation of MOF@SiO 2 Core-shell microsphere HPLC chiral column (column A), the specific method is:

[0022] (1) Chiral [Co 2 (D-cam) 2 (TMDPy)]@SiO 2 Synthesis of core-shell composites: 100 mL of deionized water was added to a round bottom flask, and 0.7205 g of Co(CH 3 COO) 2 4H 2 O and 1.0693 g aminopropylated SiO 2 The microspheres were stirred at room temperature for 30 min, filtered, and washed 3 times with deionized water. Add the filter residue to a round-bottomed flask, and add 100 mL of deionized water, 0.5854 g of D-camphoric acid, 0.5750 g of 1,3-di(4-pyridyl)propane, 0.3295 g of anhydrous potassium carbonate, and then reflux at 110°C React for 6 days and cool to room temperature. filter, the resulting [Co 2 (D-cam) 2 (TMDPy)]@SiO 2 The microspheres were washed 6 times with deionized water and absolute ethanol respectively, used as the stationary phase, and dried for later use. (See figure 2 )

[0023] (2) Filling of chiral column: Weigh...

Embodiment 2

[0036] A good HPLC chiral column usually has good reproducibility and stability. In order to examine the reproducibility and stability of column A, using n-hexane / isopropanol (9:1, V / V) as the mobile phase, trans-1,2-diphenyloxirane was continuously injected for 5 Second-rate. Depend on Figure 4 It can be seen that the chiral MOF@SiO 2 The resolution effect of the column on trans-1,2-diphenyloxirane remained basically unchanged, and the relative standard deviation (RSD) of its retention time (n=5) and peak area were 0.47% and 1.38%, respectively, It shows that the chiral MOF@SiO of the present invention 2 The column has good stability and reproducibility.

[0037] Figure 5 are racemic compounds respectively in MOF@SiO 2 Schematic diagram of the comparison of split results on column and MOF column, by Figure 5 It can be seen that pure MOF[Co 2 (D-cam) 2 (TMDPy)] crystals are irregular in shape and particles are not uniform, and the column efficiency obtained by pack...

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Abstract

The invention discloses an MOF@SiO2 core-shell microsphere HPLC chiral column for enantiomeric resolution. A method of in-situ growth is used, aminopropyl silica gel is used as a core, and chiral MOFscontrollably grow on the surface of the core as a shell to synthesize a core-shell composite material, and the MOF@SiO2 core-shell microsphere is used as a high performance liquid chromatography stationary phase for chiral separation. Compared with a pure MOF chiral column, the MOF@SiO2 core-shell microsphere HPLC chiral column of the invention can resolve multiple enantiomers, and the chromatographic column has many advantages of higher resolution, higher column efficiency and faster separation speed, which is of great significance to improve the problems of high background pressure and lowcolumn efficiency of a pure crystal column caused by uneven crystal particles.

Description

technical field [0001] The invention belongs to the technical field of high-performance liquid chromatography chiral separation, and specifically relates to a MOF prepared from a core-shell composite material prepared with aminopropyl silica gel as a core and a chiral metal-organic framework as a shell as a stationary phase of high performance liquid chromatography @SiO 2 Core-shell microsphere HPLC chiral column. Background technique [0002] Metal-organic frameworks (MOFs) are porous ligands with one-dimensional or multi-dimensional periodic network structures obtained by transition metal ions or metal clusters and organic multidentate ligands through molecular self-assembly and crystal engineering. bit polymer. In recent years, the development of MOFs materials has been very rapid, and they have been widely used in the fields of gas adsorption, molecular separation, catalysis, sensing and drug release. [0003] So far, a large number of chiral MOFs materials have been ...

Claims

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Application Information

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IPC IPC(8): B01D15/22B01J20/22B01J20/29B01J20/30
CPCB01D15/22B01J20/103B01J20/226B01J20/29
Inventor 谢生明袁宝燕李丽
Owner YUNNAN NORMAL UNIV
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