<p>A&#xa0;chiral core–shell microsphere composite, L-His-ZIF-67@SiO<sub>2</sub>, was constructed by a one-pot method using SiO<sub>2</sub>-COOH as the carrier. The density of the MOF shell was regulated by altering the reaction time and the mixing ratio of the precursor to SiO<sub>2</sub>-COOH. As a new chiral stationary phase (CSP), the core–shell composite was applied to the&#xa0; enantiomeric separation in HPLC. With n-hexane/isopropanol as the mobile phase, a great variety of positional isomers and racemates were separated on the L-His-ZIF-67@SiO<sub>2</sub> packed column. There are 6 positional isomers and 12 chiral compounds including alcohols, ketones, epoxides, and esters that can be separated on this chiral column with good separation efficiency. The separation performance of the chiral column was examined in relation to injection masses, temperature, and mobile phase composition. Its application in the determination of enantiomeric excess and isomeric impurities in actual samples demonstrated its feasibility for practical HPLC analysis. Additionally, the chiral resolution capabilities of the L-His-ZIF-67@SiO<sub>2</sub> packed column were compared with those of two commercial chiral columns, indicating that the L-His-ZIF-67@SiO<sub>2</sub> packed column can serve as a complementary alternative. The results demonstrate that optimizing reaction conditions to construct uniform chiral MOFs@SiO<sub>2</sub> composites for HPLC enantioseparation offers novel insights into the development of MOF materials in chromatography.</p> Graphical Abstract <p></p>

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Facile one-pot preparation of chiral metal–organic framework L-His-ZIF-67@SiO2 composite for HPLC enantioseparation

  • Ren-Xiu He,
  • Hao Wang,
  • Tian-Jian Xiong,
  • Yun-Qiao Zhao,
  • Yun-Jie Li,
  • Bang-Jin Wang,
  • Jun-Hui Zhang,
  • Sheng-Ming Xie,
  • Jia-Ni Yang,
  • Li-Ming Yuan

摘要

A chiral core–shell microsphere composite, L-His-ZIF-67@SiO2, was constructed by a one-pot method using SiO2-COOH as the carrier. The density of the MOF shell was regulated by altering the reaction time and the mixing ratio of the precursor to SiO2-COOH. As a new chiral stationary phase (CSP), the core–shell composite was applied to the  enantiomeric separation in HPLC. With n-hexane/isopropanol as the mobile phase, a great variety of positional isomers and racemates were separated on the L-His-ZIF-67@SiO2 packed column. There are 6 positional isomers and 12 chiral compounds including alcohols, ketones, epoxides, and esters that can be separated on this chiral column with good separation efficiency. The separation performance of the chiral column was examined in relation to injection masses, temperature, and mobile phase composition. Its application in the determination of enantiomeric excess and isomeric impurities in actual samples demonstrated its feasibility for practical HPLC analysis. Additionally, the chiral resolution capabilities of the L-His-ZIF-67@SiO2 packed column were compared with those of two commercial chiral columns, indicating that the L-His-ZIF-67@SiO2 packed column can serve as a complementary alternative. The results demonstrate that optimizing reaction conditions to construct uniform chiral MOFs@SiO2 composites for HPLC enantioseparation offers novel insights into the development of MOF materials in chromatography.

Graphical Abstract