The uniform zirconia nanoparticle multilayers/micrometer-sized silica particle(ZrO 2/SiO 2) was prepared for HPLC support material by layer-by-layer(LbL) self-assembly technique. XRD pattern shows that the crystalline...The uniform zirconia nanoparticle multilayers/micrometer-sized silica particle(ZrO 2/SiO 2) was prepared for HPLC support material by layer-by-layer(LbL) self-assembly technique. XRD pattern shows that the crystalline of nanometer particles on the surface is pure tetragonal zirconia, with a diameter of 13^9 nm. The specific surface area, pore volume and pore size of the material are 172.53 m 2/g, 0.378 4 cm 3/g, and 8.5 nm, respectively. The novel support not only has the mechanical strength and chemical stability of zirconia, but also has the good chromatographic features such as larger surface area, better permeability, less background pressure.展开更多
The surface properties of zirconia-based supports,ZrO-2/SiO-2 and ZrO-2,were compared.ZrO-2/SiO-2 prepared by layer-by-layer self-assembly(LbL SA) technique showed more favorable characteristics for HPLC applications ...The surface properties of zirconia-based supports,ZrO-2/SiO-2 and ZrO-2,were compared.ZrO-2/SiO-2 prepared by layer-by-layer self-assembly(LbL SA) technique showed more favorable characteristics for HPLC applications compared with ZrO-2 prepared by modified oil-emulsion method.The specific surface area and pore volume of ZrO-2/SiO-2 were about 18 and 20 times of those of ZrO-2 respectively.The pore of ZrO-2/SiO-2 support was ideal cylindrical shape,but ZrO-2 support had some \!ink bottle\" shaped-pores which was unfavorable for HPLC separations.Pore size distribution of ZrO-2/SiO-2 supports was more uniform than that of ZrO-2 supports.展开更多
A low cost,rapid and sensitive preparation method of silica gel supported ionic liquid(SGSIL)combined with matrix solid phase dispersion(MSPD)followed by high performance liquid chromatography(HPLC)with ultraviolet de...A low cost,rapid and sensitive preparation method of silica gel supported ionic liquid(SGSIL)combined with matrix solid phase dispersion(MSPD)followed by high performance liquid chromatography(HPLC)with ultraviolet detection(UV)is proposed,and it was applied to determine the seven active compounds in Salvia Miltiorrhiza herb.SGSIL and ionic liquid[BMIM]BF4 were used as the adsorbent and the green elution reagent in the MSPD procedure.Several extraction conditions including type of filler and elution solvent,the volume of elution solvent,material liquid ratio were optimized.Under the optimum conditions,the SGSIL-MSPD-HPLC method showed a low limit of detection(LOD,S/N=3)of 0.0122-0.8788μg/mL for standard solution,limit of quantification(LOQ,S/N=10)of 0.0406-2.9292μg/mL for standard solution,wide linear range from 1.56 to 2000μg/mL for all compounds for standard solution,correlation coefficients(r)of more than 0.9990,acceptable reproducibility(relative standard deviations,RSDs<3.54%),and precision of RSDs<3.36%for intra-day,RSDs<3.50%for inter-day.The satisfactory recoveries ranged from 96.4 to 102.5,with RSDs less than 3.45%.The developed SGSIL-MSPD method is easier and more suitable for the determination of the seven active compounds in Salvia Miltiorrhiza herb than the traditional ultrasonic extraction.It was an effective and efficient method for the extraction and quantification of the seven active compounds in traditional Chinese herbal samples.展开更多
文摘The uniform zirconia nanoparticle multilayers/micrometer-sized silica particle(ZrO 2/SiO 2) was prepared for HPLC support material by layer-by-layer(LbL) self-assembly technique. XRD pattern shows that the crystalline of nanometer particles on the surface is pure tetragonal zirconia, with a diameter of 13^9 nm. The specific surface area, pore volume and pore size of the material are 172.53 m 2/g, 0.378 4 cm 3/g, and 8.5 nm, respectively. The novel support not only has the mechanical strength and chemical stability of zirconia, but also has the good chromatographic features such as larger surface area, better permeability, less background pressure.
文摘The surface properties of zirconia-based supports,ZrO-2/SiO-2 and ZrO-2,were compared.ZrO-2/SiO-2 prepared by layer-by-layer self-assembly(LbL SA) technique showed more favorable characteristics for HPLC applications compared with ZrO-2 prepared by modified oil-emulsion method.The specific surface area and pore volume of ZrO-2/SiO-2 were about 18 and 20 times of those of ZrO-2 respectively.The pore of ZrO-2/SiO-2 support was ideal cylindrical shape,but ZrO-2 support had some \!ink bottle\" shaped-pores which was unfavorable for HPLC separations.Pore size distribution of ZrO-2/SiO-2 supports was more uniform than that of ZrO-2 supports.
基金This research was supported by Special Research Fund for Young Doctors of Qiqihar Medical University(QMSI2020B-03,hosted by Wenjing Li).
文摘A low cost,rapid and sensitive preparation method of silica gel supported ionic liquid(SGSIL)combined with matrix solid phase dispersion(MSPD)followed by high performance liquid chromatography(HPLC)with ultraviolet detection(UV)is proposed,and it was applied to determine the seven active compounds in Salvia Miltiorrhiza herb.SGSIL and ionic liquid[BMIM]BF4 were used as the adsorbent and the green elution reagent in the MSPD procedure.Several extraction conditions including type of filler and elution solvent,the volume of elution solvent,material liquid ratio were optimized.Under the optimum conditions,the SGSIL-MSPD-HPLC method showed a low limit of detection(LOD,S/N=3)of 0.0122-0.8788μg/mL for standard solution,limit of quantification(LOQ,S/N=10)of 0.0406-2.9292μg/mL for standard solution,wide linear range from 1.56 to 2000μg/mL for all compounds for standard solution,correlation coefficients(r)of more than 0.9990,acceptable reproducibility(relative standard deviations,RSDs<3.54%),and precision of RSDs<3.36%for intra-day,RSDs<3.50%for inter-day.The satisfactory recoveries ranged from 96.4 to 102.5,with RSDs less than 3.45%.The developed SGSIL-MSPD method is easier and more suitable for the determination of the seven active compounds in Salvia Miltiorrhiza herb than the traditional ultrasonic extraction.It was an effective and efficient method for the extraction and quantification of the seven active compounds in traditional Chinese herbal samples.
