Zwitterionic sulfobetaine-based monolithic stationary phases have attracted increasing attention for their use in hydrophilic interaction chromatography.In this study,a novel hydrophilic polymeric monolith was fabrica...Zwitterionic sulfobetaine-based monolithic stationary phases have attracted increasing attention for their use in hydrophilic interaction chromatography.In this study,a novel hydrophilic polymeric monolith was fabricated through photo-initiated copolymerization of 3-(3-vinyl-1-imidazolio)-1-propanesulfonate(SBVI)with pentaerythritol triacrylate using methanol and tetrahydrofuran as the porogenic system.Notably,the duration for the preparation of this novel monolith was as little as 5 min,which was significantly shorter than that required for previously reported sulfobetaine-based monoliths prepared via conventional thermally initiated copolymerization.Moreover,these monoliths showed good morphology,permeability,porosity(62.4%),mechanical strength(over 15 MPa),column efficiency(51,230 plates/m),and reproducibility(relative standard deviations for all analytes were lower than 4.6%).Mechanistic studies indicated that strong hydrophilic and negative electrostatic interactions might be responsible for the retention of polar analytes on the zwitterionic SBVI-based monolith.In particular,the resulting monolith exhibited good anti-protein adhesion ability and low nonspecific protein adsorption.These excellent features seem to favor its application in bioanalysis.Therefore,the novel zwitterionic sulfobetaine-based monolith was successfully employed for the highly selective separation of small bioactive compounds and the efficient enrichment of N-glycopeptides from complex samples.In this study,we prepared a novel zwitterionic sulfobetaine-based monolith with good performance and developed a simpler and faster method for preparation of zwitterionic monoliths.展开更多
Aryloxypropanolamine is an essential structural scaffold for a variety of b-adrenergic receptor antagonists such as metoprolol.Molecules with such a structural motif tend to degrade into α,β ehydroxypropanolamine im...Aryloxypropanolamine is an essential structural scaffold for a variety of b-adrenergic receptor antagonists such as metoprolol.Molecules with such a structural motif tend to degrade into α,β ehydroxypropanolamine impurities via a radicaleinitiated oxidation pathway.These impurities are typically polar and nonchromophoric,and are thus often overlooked using traditional reversed phase chromatography and UV detection.In this work,stress testing of metoprolol confirmed the generation of 3-isopropylamino-1,2-propanediol as a degradation product,which is a specified impurity of metoprolol in the European Pharmacopoeia(impurity N).To ensure the safety and quality of metoprolol drug products,hydrophilic interaction chromatography(HILIC)methods using Halo Penta HILIC column(150mm×4.6 mm,5 μm)coupled with charged aerosol detection(CAD)were developed and optimized for the separation and quantitation of metoprolol impurity N in metoprolol drug products including metoprolol tartrate injection,metoprolol tartrate tablets,and metoprolol succinate extended-release tablets.These HILIC-CAD methods were validated per USP validation guidelines with respect to specificity,linearity,accuracy,and precision,and have been successfully applied to determine impurity N in metoprolol drug products.展开更多
Porous graphene(PG) has potential applications in numerous fields because of the existence of nanopores in the plane. In this study, porous graphene decorated silica microspheres(Sil-PG) were successfully fabricated b...Porous graphene(PG) has potential applications in numerous fields because of the existence of nanopores in the plane. In this study, porous graphene decorated silica microspheres(Sil-PG) were successfully fabricated by assembling PG onto the silica particles surface in deep eutectic solvents(DESs).Experimental results demonstrate that this new stationary phase can facilitate the separation of six sulfonamides compounds in hydrophilic chromatographic conditions. The successful synthesis of the SilPG stationary phase provides a basis for the application of porous graphene-modified materials as the stationary phase for liquid chromatography, and offers the possibility to broaden the application of PG in the field of chromatography.展开更多
A one-step procedure to hydrophilize monodisperse poly（chloromethyl-styrene-co-divinylbenzene） beads has been presented with 2-hydroxy-3-[4-（hydroxymethyl）-1H-1,2,3-triazol-1-yl]propy1 2-methylacrylate（HTMA） as ...A one-step procedure to hydrophilize monodisperse poly（chloromethyl-styrene-co-divinylbenzene） beads has been presented with 2-hydroxy-3-[4-（hydroxymethyl）-1H-1,2,3-triazol-1-yl]propy1 2-methylacrylate（HTMA） as monomer by surface-initiated atom transfer radical polymerization（SI-ATRP）.The length of the grafted poly（HTMA） chain was varied via controlling the ratio of HTMA to initiator on the surface of the beads.Using these grafted beads as the stationary phase in hydrophilic interaction chromatography,good separation was obtained for nucleosides in the mobile phase of acetonitrile-water.It was also found that the retention time and selectivity of solutes showed a positive relationship with the length of the grafted poly（HTMA） chain.展开更多
基金supported by the National Natural Science Foundation of China(Grant Nos.:82173773 and 82073806)the Natural Science Foundation of Guangdong Province,China(Grant Nos.:2020A1515010569 and 2021A0505030039)Science and Technology Program of Guangzhou,China(Grant No.:202102020729).
文摘Zwitterionic sulfobetaine-based monolithic stationary phases have attracted increasing attention for their use in hydrophilic interaction chromatography.In this study,a novel hydrophilic polymeric monolith was fabricated through photo-initiated copolymerization of 3-(3-vinyl-1-imidazolio)-1-propanesulfonate(SBVI)with pentaerythritol triacrylate using methanol and tetrahydrofuran as the porogenic system.Notably,the duration for the preparation of this novel monolith was as little as 5 min,which was significantly shorter than that required for previously reported sulfobetaine-based monoliths prepared via conventional thermally initiated copolymerization.Moreover,these monoliths showed good morphology,permeability,porosity(62.4%),mechanical strength(over 15 MPa),column efficiency(51,230 plates/m),and reproducibility(relative standard deviations for all analytes were lower than 4.6%).Mechanistic studies indicated that strong hydrophilic and negative electrostatic interactions might be responsible for the retention of polar analytes on the zwitterionic SBVI-based monolith.In particular,the resulting monolith exhibited good anti-protein adhesion ability and low nonspecific protein adsorption.These excellent features seem to favor its application in bioanalysis.Therefore,the novel zwitterionic sulfobetaine-based monolith was successfully employed for the highly selective separation of small bioactive compounds and the efficient enrichment of N-glycopeptides from complex samples.In this study,we prepared a novel zwitterionic sulfobetaine-based monolith with good performance and developed a simpler and faster method for preparation of zwitterionic monoliths.
文摘Aryloxypropanolamine is an essential structural scaffold for a variety of b-adrenergic receptor antagonists such as metoprolol.Molecules with such a structural motif tend to degrade into α,β ehydroxypropanolamine impurities via a radicaleinitiated oxidation pathway.These impurities are typically polar and nonchromophoric,and are thus often overlooked using traditional reversed phase chromatography and UV detection.In this work,stress testing of metoprolol confirmed the generation of 3-isopropylamino-1,2-propanediol as a degradation product,which is a specified impurity of metoprolol in the European Pharmacopoeia(impurity N).To ensure the safety and quality of metoprolol drug products,hydrophilic interaction chromatography(HILIC)methods using Halo Penta HILIC column(150mm×4.6 mm,5 μm)coupled with charged aerosol detection(CAD)were developed and optimized for the separation and quantitation of metoprolol impurity N in metoprolol drug products including metoprolol tartrate injection,metoprolol tartrate tablets,and metoprolol succinate extended-release tablets.These HILIC-CAD methods were validated per USP validation guidelines with respect to specificity,linearity,accuracy,and precision,and have been successfully applied to determine impurity N in metoprolol drug products.
基金Financial supports from the National Natural Science Foundation of China (Nos. 21822407 and 21675164)the funds for Distinguished Young Scientists of Gansu (No. 1506RJDA281) are gratefully acknowledged
文摘Porous graphene(PG) has potential applications in numerous fields because of the existence of nanopores in the plane. In this study, porous graphene decorated silica microspheres(Sil-PG) were successfully fabricated by assembling PG onto the silica particles surface in deep eutectic solvents(DESs).Experimental results demonstrate that this new stationary phase can facilitate the separation of six sulfonamides compounds in hydrophilic chromatographic conditions. The successful synthesis of the SilPG stationary phase provides a basis for the application of porous graphene-modified materials as the stationary phase for liquid chromatography, and offers the possibility to broaden the application of PG in the field of chromatography.
基金supported by National Natural Science Foundation of China(No.20975080)Program for New Century Excellent Talents in University(No.NCET-08-0892)+1 种基金Major State Basic Research Development Program of China(No.2009CB26608)Natural Science Foundation of Ningxia Province(No.NZ0914)
文摘A one-step procedure to hydrophilize monodisperse poly（chloromethyl-styrene-co-divinylbenzene） beads has been presented with 2-hydroxy-3-[4-（hydroxymethyl）-1H-1,2,3-triazol-1-yl]propy1 2-methylacrylate（HTMA） as monomer by surface-initiated atom transfer radical polymerization（SI-ATRP）.The length of the grafted poly（HTMA） chain was varied via controlling the ratio of HTMA to initiator on the surface of the beads.Using these grafted beads as the stationary phase in hydrophilic interaction chromatography,good separation was obtained for nucleosides in the mobile phase of acetonitrile-water.It was also found that the retention time and selectivity of solutes showed a positive relationship with the length of the grafted poly（HTMA） chain.
