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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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 so

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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[0020] Example 1

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

[0022] (1) Chirality (Co 2 (D-cam) 2 (TMDPy)]@SiO 2 Synthesis of core-shell composite material: 100mL deionized water was added to a round bottom flask, and 0.7205g Co(CH 3 COO) 2 ·4H 2 O and 1.0693g aminopropylated SiO 2 The microspheres were stirred at room temperature for 30 minutes, filtered, and washed with deionized water three times. Put the filter residue into a round bottom flask, and add 100mL deionized water, 0.5854g D-camphoric acid, 0.5750g 1,3-bis(4-pyridyl)propane, 0.3295g anhydrous potassium carbonate, and then reflux at 110℃ React for 6 days and cool to room temperature. Filter, the [Co 2 (D-cam) 2 (TMDPy)]@SiO 2 The microspheres were washed with deionized water and absolute ethanol for 6 times, used as a stationary phase, and dried for later use. (see figure 2 )

[0023] (2) Packing of chiral column: Weigh 1.2g of prepared chiral ...

Example Embodiment

[0035] Example 2

[0036] An excellent chiral column for high performance liquid chromatography usually has good reproducibility and stability. In order to investigate the reproducibility and stability of column A, n-hexane / isopropanol (9:1, V / V) was used as the mobile phase, and trans-1,2-diphenylethylene oxide was continuously injected 5 Times. by Figure 4 It can be seen that the chiral MOF@SiO 2 The resolution of trans-1,2-diphenyloxirane by the column remained basically unchanged, and the retention time (n=5) and the relative standard deviation (RSD) of the peak area were 0.47% and 1.38%, respectively. Shows the chiral MOF@SiO of the present invention 2 The column has good stability and reproducibility.

[0037] Figure 5 Are racemic compounds in MOF@SiO 2 Schematic diagram of the comparison of the splitting results on the column and the MOF column. Figure 5 It can be seen that pure MOF[Co 2 (D-cam) 2 (TMDPy)] The crystal shape is irregular and the particles are not unifo...

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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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