Titania microspheres were synthesized using hydrothermal methods to exploit a new liquid chromatography stationary phase. The prepared titania microspheres were approximately 7 μm in diameter, and the particle size d...Titania microspheres were synthesized using hydrothermal methods to exploit a new liquid chromatography stationary phase. The prepared titania microspheres were approximately 7 μm in diameter, and the particle size distribution was relatively narrow and uniform. Furthermore, the average specific surface area was 276.0 m2·g·1, the average pore volume was approximately 0.25 mL·g·1, and the pore diameter was approximately 35.9 nm for sintering titania microspheres. These parameters indicate that the titania microspheres prepared for this study have excellent surface properties for chromatography. Additionally, columns filled with the titania microspheres were able to separate basic compounds, including benzene, nitrobenzene and o-nitroanisole. It could be proposed that the titania microspheres prepared for this study would be a promising stationary phase for liquid chromatography.展开更多
Ionic liquids（ILs） immobilized on silica as novel high performance liquid chromatography（HPLC）stationary phases have attracted considerable attention. However, it has not been applied to protein separation. In thi...Ionic liquids（ILs） immobilized on silica as novel high performance liquid chromatography（HPLC）stationary phases have attracted considerable attention. However, it has not been applied to protein separation. In this paper, N-methylimidazolium IL-modified silica-based stationary phase（Silpr Mim）was prepared and investigated as a novel multi-interaction stationary phase charged positively for protein separation. The results indicate that all of the basic proteins tested cannot be absorbed on this novel stationary phase, whereas all of the acidic proteins tested can be retained, and the baseline separation of eight kinds of acidic protein standards can be achieved when performed in reversed phase/ion-exchange chromatography（RPLC/IEC） mode. Compared with commonly used commercial octadecylated silica（ODS） column, the novel stationary phase can show selectivity and good resolution to acidic proteins, which has a promising application in the separation and analyses of acidic proteins from the complex samples in proteomics. In addition, the chromatographic behavior of proteins, the effect of the ligand structure and the retention mechanism on this stationary phase were also investigated.展开更多
In this paper,the concept of reversed-or normal-phase chiral stationary phase liquid chromatography has been put forward according to the polar strength of mobile and stationary phases. The statistical model developed...In this paper,the concept of reversed-or normal-phase chiral stationary phase liquid chromatography has been put forward according to the polar strength of mobile and stationary phases. The statistical model developed in HPLC has been used to investigate the separation mechanism of D-and L-enantiomer in chiral stationary phase liquid chromatography.It has been observed that the variation of capacity factor of enantiomers with mobile phase composition in both reversed-phase and normal-phase chiral stationary phase liquid chromatography can be described by the fundamental elution equation lnk'=a+blnC_b+cC_b.The effect of mobile phase composition on the selec- tivity of enantiomers D and L in normal-phase chiral stationary phase liquid chromatography cam be described by the equation lnα=⊿a+⊿blnC_b,but in reversed-phase chiral stationary phase liquid chromatography the selectivity is almost independant of the mobile phase composition.展开更多
文摘Titania microspheres were synthesized using hydrothermal methods to exploit a new liquid chromatography stationary phase. The prepared titania microspheres were approximately 7 μm in diameter, and the particle size distribution was relatively narrow and uniform. Furthermore, the average specific surface area was 276.0 m2·g·1, the average pore volume was approximately 0.25 mL·g·1, and the pore diameter was approximately 35.9 nm for sintering titania microspheres. These parameters indicate that the titania microspheres prepared for this study have excellent surface properties for chromatography. Additionally, columns filled with the titania microspheres were able to separate basic compounds, including benzene, nitrobenzene and o-nitroanisole. It could be proposed that the titania microspheres prepared for this study would be a promising stationary phase for liquid chromatography.
基金supported by the National 863 Program(No.2006AA02Z227)Natural Science Foundation of Shaanxi Province(No.2011JZ002)+1 种基金the Foundation of Key Laboratory in Shaanxi Province(Nos.2010JS103,11JS097,14JS098)Shaanxi Provincial Science and Technology Co-ordinating innovation projects(No.2013SZS18-K01)
文摘Ionic liquids（ILs） immobilized on silica as novel high performance liquid chromatography（HPLC）stationary phases have attracted considerable attention. However, it has not been applied to protein separation. In this paper, N-methylimidazolium IL-modified silica-based stationary phase（Silpr Mim）was prepared and investigated as a novel multi-interaction stationary phase charged positively for protein separation. The results indicate that all of the basic proteins tested cannot be absorbed on this novel stationary phase, whereas all of the acidic proteins tested can be retained, and the baseline separation of eight kinds of acidic protein standards can be achieved when performed in reversed phase/ion-exchange chromatography（RPLC/IEC） mode. Compared with commonly used commercial octadecylated silica（ODS） column, the novel stationary phase can show selectivity and good resolution to acidic proteins, which has a promising application in the separation and analyses of acidic proteins from the complex samples in proteomics. In addition, the chromatographic behavior of proteins, the effect of the ligand structure and the retention mechanism on this stationary phase were also investigated.
基金This work was supported by the National Natural Science Foundation of China.
文摘In this paper,the concept of reversed-or normal-phase chiral stationary phase liquid chromatography has been put forward according to the polar strength of mobile and stationary phases. The statistical model developed in HPLC has been used to investigate the separation mechanism of D-and L-enantiomer in chiral stationary phase liquid chromatography.It has been observed that the variation of capacity factor of enantiomers with mobile phase composition in both reversed-phase and normal-phase chiral stationary phase liquid chromatography can be described by the fundamental elution equation lnk'=a+blnC_b+cC_b.The effect of mobile phase composition on the selec- tivity of enantiomers D and L in normal-phase chiral stationary phase liquid chromatography cam be described by the equation lnα=⊿a+⊿blnC_b,but in reversed-phase chiral stationary phase liquid chromatography the selectivity is almost independant of the mobile phase composition.
