Capillary electrochromatography(CEC)plays a significant role in chiral separation via the double separation principle,partition coefficient difference between the two phases,and electroosmotic flow-driven separation.G...Capillary electrochromatography(CEC)plays a significant role in chiral separation via the double separation principle,partition coefficient difference between the two phases,and electroosmotic flow-driven separation.Given the distinct properties of the inner wall stationary phase(SP),the separation ability of each SP differs from one another.Particularly,it provides large room for promising applications of open tubular capillary electrochromatography(OT-CEC).We divided the OT-CEC SPs developed over the past four years into six types:ionic liquids,nanoparticle materials,microporous materials,biomaterials,non-nanopolymers,and others,to mainly introduce their characteristics in chiral drug separation.There also added a few classic SPs that occurred within ten years as supplements to enrich the features of each SP.Additionally,we discuss their applications in metabolomics,food,cosmetics,environment,and biology as analytes in addition to chiral drugs.OT-CEC plays an increasingly significant role in chiral separation and may promote the development of capillary electrophoresis(CE)combined with other instruments in recent years,such as CE with mass spectrometry(CE/MS)and CE with ultraviolet light detector(CE/UV).展开更多
Capillary chromatography using an untreated open tubular capillary tube and a ternary solvent mixture consisting of water-hydrophilic/hydrophobic organic solvent as a carrier solution has been developed. The system is...Capillary chromatography using an untreated open tubular capillary tube and a ternary solvent mixture consisting of water-hydrophilic/hydrophobic organic solvent as a carrier solution has been developed. The system is called tube radical distribution chromatography (TRDC). Separation performance of the TRDC system using a fused-silica capillary tube was examined through the phase diagram for the ternary water-acetonitrile-ethyl acetate solvent mixture. The TRDC system required homogeneous carrier solutions with solvent component ratios around the boundary curve between homogeneous and heterogeneous solution in the phase diagram. The data obtained using the fused-silica capillary tube were compared with those obtained using a polytetrafluoroethylene capillary tube in our previous study.展开更多
In this wo rk,the phase-transitioned BSA(PTB)film using the mild and fast fabrication process adhered to the capillary inner wall uniformly,and the fabricated PTB film-coated capillary column was applied to realize op...In this wo rk,the phase-transitioned BSA(PTB)film using the mild and fast fabrication process adhered to the capillary inner wall uniformly,and the fabricated PTB film-coated capillary column was applied to realize open tubular capillary electrochromatography(OT-CEC)enantioseparation.The enantioseparation ability of PTB film-coated capillary was evaluated with eight pairs of chiral analytes including drugs and neurotransmitters,all achieving good resolution and symmetrical peak shape.For three consecutive runs,the relative standard deviations(RSD)of migration time for intra-day,inter-day,and column-tocolumn repeatability were in the range of 0.3%-3.5%,0.2%-4.9%and 2.1%-7.7%,respectively.Moreover,the PTB film-coated capillary column ran continuously over 300 times with high separation efficiency.Therefore,the coating method based on BSA self-assembly supramolecular film can be extended to the preparation of other proteinaceous capillary columns.展开更多
A new open-tubular capillary electrochromatography (OT-CEC) method for analysis of β-lactam antibiotics has been developed with unique block co-polymer coating. To obtain the highly ordered block polymer chains, reve...A new open-tubular capillary electrochromatography (OT-CEC) method for analysis of β-lactam antibiotics has been developed with unique block co-polymer coating. To obtain the highly ordered block polymer chains, reversible addition fragmentation chain transfer radical polymerization method was used to synthesize poly (maleic anhydride-styrene-N-isopropylacrylamide). The prepared block copolymer coating was characterized with NMR, fourier transform infrared spectroscopy and scanning electron microscope. Several key separation factors of OT-CEC, which including polymer amount,stability of the coating, temperature, species of organic additives, buffer pH and concentration, were investigated in detail. Our results indicated that the separation efficiency was improved greatly with the coating capillary and the three test analytes could be baseline separated. Then, the separation mechanism was briefly explored. Moreover, the proposed OT-CEC method displayed promising quantitative analysis property of the three test analytes with good linearity (R2>0.99), repeatability (relative standard deviations <0.9%) and high recovery (95.4%-106.2%). Further, the assay was applied in monitoring the three test β-lactam antibiotics (cephradine, cephalexin and amoxicillin) in serum samples, providing a useful platform for construction of novel polymer coatings in OT-CEC system and for analysis of drugs in real bio-samples.展开更多
This paper covers the preparation of a sol gel derived macrocyclic dioxopolyamine(1,4,7,10 tetraazaclotridecane 11,13 dione) stationary phase for open tubular capillary electrochromatography(OTCEC). The sol gel derive...This paper covers the preparation of a sol gel derived macrocyclic dioxopolyamine(1,4,7,10 tetraazaclotridecane 11,13 dione) stationary phase for open tubular capillary electrochromatography(OTCEC). The sol gel derived macrocyclic dioxopolyamine capillary columns have shown improved separations of neurotransmitters, isomeric nitrophenols, isomeric dihydroxybenzenes, isomeric aminophenols, isomeric diaminobenzenes and three ortho halogen anilines, in comparison with those of untreated capillaries. The characteristics of the sol gel derived macrocyclic dioxopolyamine capillary columns are compared with the capillary column modified with the macrocyclic dioxopolyamine by chemically bonded method after etching. The sol gel method provided a porous silica material with stationary phase in place within the same experimental procedure. This provided speedy fabrications of high efficiency columns with high surface area and improved phase ratio. We achieved high efficiencies of 60 000-340 000 plates/m for the various isomeric compounds. The reproducibility migration time and the plate number were pretty good.展开更多
基金This study was funded by the Project of National Natural Science Foundation of China(Grant No.:82003705)the Shanghai Science and Technology Innovation Foundation(Grant Nos.:23010500200 and 23ZR1422700).
文摘Capillary electrochromatography(CEC)plays a significant role in chiral separation via the double separation principle,partition coefficient difference between the two phases,and electroosmotic flow-driven separation.Given the distinct properties of the inner wall stationary phase(SP),the separation ability of each SP differs from one another.Particularly,it provides large room for promising applications of open tubular capillary electrochromatography(OT-CEC).We divided the OT-CEC SPs developed over the past four years into six types:ionic liquids,nanoparticle materials,microporous materials,biomaterials,non-nanopolymers,and others,to mainly introduce their characteristics in chiral drug separation.There also added a few classic SPs that occurred within ten years as supplements to enrich the features of each SP.Additionally,we discuss their applications in metabolomics,food,cosmetics,environment,and biology as analytes in addition to chiral drugs.OT-CEC plays an increasingly significant role in chiral separation and may promote the development of capillary electrophoresis(CE)combined with other instruments in recent years,such as CE with mass spectrometry(CE/MS)and CE with ultraviolet light detector(CE/UV).
文摘Capillary chromatography using an untreated open tubular capillary tube and a ternary solvent mixture consisting of water-hydrophilic/hydrophobic organic solvent as a carrier solution has been developed. The system is called tube radical distribution chromatography (TRDC). Separation performance of the TRDC system using a fused-silica capillary tube was examined through the phase diagram for the ternary water-acetonitrile-ethyl acetate solvent mixture. The TRDC system required homogeneous carrier solutions with solvent component ratios around the boundary curve between homogeneous and heterogeneous solution in the phase diagram. The data obtained using the fused-silica capillary tube were compared with those obtained using a polytetrafluoroethylene capillary tube in our previous study.
基金the financial support from the National Natural Science Foundation of China(No.21874060)the Special Funding for Open and Shared Large-Scale Instruments and Equipments of Lanzhou University(No.LZU-GXJJ-2019C038)。
文摘In this wo rk,the phase-transitioned BSA(PTB)film using the mild and fast fabrication process adhered to the capillary inner wall uniformly,and the fabricated PTB film-coated capillary column was applied to realize open tubular capillary electrochromatography(OT-CEC)enantioseparation.The enantioseparation ability of PTB film-coated capillary was evaluated with eight pairs of chiral analytes including drugs and neurotransmitters,all achieving good resolution and symmetrical peak shape.For three consecutive runs,the relative standard deviations(RSD)of migration time for intra-day,inter-day,and column-tocolumn repeatability were in the range of 0.3%-3.5%,0.2%-4.9%and 2.1%-7.7%,respectively.Moreover,the PTB film-coated capillary column ran continuously over 300 times with high separation efficiency.Therefore,the coating method based on BSA self-assembly supramolecular film can be extended to the preparation of other proteinaceous capillary columns.
基金financial support from the National Natural Science Foundation of China (Nos. 21727809, 21635008, 21621062)Chinese Academy of Sciences(No. QYZDJ-SSW-SLH034)
文摘A new open-tubular capillary electrochromatography (OT-CEC) method for analysis of β-lactam antibiotics has been developed with unique block co-polymer coating. To obtain the highly ordered block polymer chains, reversible addition fragmentation chain transfer radical polymerization method was used to synthesize poly (maleic anhydride-styrene-N-isopropylacrylamide). The prepared block copolymer coating was characterized with NMR, fourier transform infrared spectroscopy and scanning electron microscope. Several key separation factors of OT-CEC, which including polymer amount,stability of the coating, temperature, species of organic additives, buffer pH and concentration, were investigated in detail. Our results indicated that the separation efficiency was improved greatly with the coating capillary and the three test analytes could be baseline separated. Then, the separation mechanism was briefly explored. Moreover, the proposed OT-CEC method displayed promising quantitative analysis property of the three test analytes with good linearity (R2>0.99), repeatability (relative standard deviations <0.9%) and high recovery (95.4%-106.2%). Further, the assay was applied in monitoring the three test β-lactam antibiotics (cephradine, cephalexin and amoxicillin) in serum samples, providing a useful platform for construction of novel polymer coatings in OT-CEC system and for analysis of drugs in real bio-samples.
文摘This paper covers the preparation of a sol gel derived macrocyclic dioxopolyamine(1,4,7,10 tetraazaclotridecane 11,13 dione) stationary phase for open tubular capillary electrochromatography(OTCEC). The sol gel derived macrocyclic dioxopolyamine capillary columns have shown improved separations of neurotransmitters, isomeric nitrophenols, isomeric dihydroxybenzenes, isomeric aminophenols, isomeric diaminobenzenes and three ortho halogen anilines, in comparison with those of untreated capillaries. The characteristics of the sol gel derived macrocyclic dioxopolyamine capillary columns are compared with the capillary column modified with the macrocyclic dioxopolyamine by chemically bonded method after etching. The sol gel method provided a porous silica material with stationary phase in place within the same experimental procedure. This provided speedy fabrications of high efficiency columns with high surface area and improved phase ratio. We achieved high efficiencies of 60 000-340 000 plates/m for the various isomeric compounds. The reproducibility migration time and the plate number were pretty good.
