Facile preparation of embedded polar group-containing pentafluorophenyl stationary phases for highly selective separations of diverse analytes.

Pentafluorophenyl (PFP) stationary phase is one of the most important phases after the C18 phase in terms of its applications. Three embedded polar groups (EPG)-containing stationary phases were newly synthesized to act the EPGs as additional interaction sites. The silica surface was initially modified with (3-aminopropyl)trimethoxysilane (APS).

Surface Modification of Silica with β-Alanine Derivatives for Unique Applications in Liquid Chromatography.

Column purchasing cost is an important issue for an analyst to analyze complex sample matrices. Here, we report the development of an amino acid (β-alanine)-derived stationary phase (Sil-Ala-C12) with strategic and effective interaction sites (amide and urea as embedded polar groups with C12 alkyl chain) able to separate various kinds of analytes. Owing to the balanced hydrophobicity and hydrophilicity of the phase, it showed exceptional separation abilities in both reversed-phase high-performance liquid chromatography (RP-HPLC) as a hydrophobic phase and hydrophilic interaction chromatography (HILIC) as a hydrophilic phase.

Design of β-Alanine-Derived Novel C18 Stationary Phase Containing Embedded Urea and Amide Groups for the Separation of Versatile Analytes.

Novel stationary phases have been emerging recently. A β-alanine-derived embedded urea and amide group-containing C18 phase (Sil-Ala-C18) was prepared for the first time. The media were packed into a 150 × 2.

Ecofriendly pretreatment of cotton fabrics by ultrasonication and reusing bath chemicals.

The textile industries of Bangladesh contribute significantly to the country's economy, accounting for more than 40% of total annual export. The quest of new technologies for efficient water and energy use in cotton knit dyeing could result in significant water savings and improve environmental sustainability. Textile wet processing consumes a lot of utilities (water and energy), and the water generates a lot of waste, which enhances chemical consumption and effluent management costs.

Progress in surface-modified silicas for Cr(VI) adsorption: A review.

Various toxic chemicals are discharging to the environment due to rapid industrialization and polluting soil, water, and air causing numerous diseases including life-threatening cancer. Among these pollutants, Cr(VI) or hexavalent chromium is one of the most carcinogenic and toxic contaminants hostile to human health and other living things. Therefore, along with other contaminants, the removal of Cr(VI) efficiently is very crucial to keep our environment neat and clean.

Remarkable enhancement of thermal stability of epoxy resin through the incorporation of mesoporous silica micro-filler.

For the first time, we incorporated mesoporous micro-silica (5 μm, pore size = 50 nm) as a filler in epoxy resin aiming to enter polymer into the pore of the silica. As expected, the thermal stability of the composite increased remarkably, followed by noteworthy thermal degradation kinetics when compared to the controlled cured epoxy resin. Composites were prepared by the direct dispersion of modified nano-silica, modified mesoporous micro-silica, unmodified mesoporous micro-silica, non-porous micro-silica, and irregular micro-silica of various pore sizes as fillers in diglycidyl ether of bisphenol-A epoxy resin via ultra-sonication and shear mixing, followed by oven-curing with 4,4-diaminodiphenyl sulfone.

Preparation of bio-inspired trimethoxysilyl group terminated poly(1-vinylimidazole)-modified-chitosan composite for adsorption of chromium (VI) ions.

Chitosan and poly(1-vinylimidazole) are both potential adsorbents to remove Cr(VI). Here, we designed the preparation of new adsorbents by combining chitosan and poly(1-vinylimidazole) to get the synergistic effect for the removal of hexavalent chromium. Trimethoxysilyl group terminated poly(1-vinylimidazole)-modified-chitosan composite was successfully synthesized by one-step free radical polymerization based on the grafting backbone of chitosan and vinylimidazole.

Facile preparation of an alternating copolymer-based high molecular shape-selective organic phase for reversed-phase liquid chromatography.

The synthesis of a new alternating copolymer-grafted silica phase is described for the separation of shape-constrained isomers of polycyclic aromatic hydrocarbons (PAHs) and tocopherols in reversed-phase high-performance liquid chromatography (RP-HPLC). Telomerization of the monomers (octadecyl acrylate and N-methylmaleimide) was carried out with a silane coupling agent; 3-mercaptopropyltrimethoxysilane (MPS), and the telomer (T) was grafted onto porous silica surface to prepare the alternating copolymer-grafted silica phase (Sil-alt-T). The new hybrid material was characterized by elemental analyses, diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy, and solid-state C and Si cross-polarization magic-angle spinning (CP/MAS) NMR spectroscopy.

Core-shell drug carrier from folate conjugated chitosan obtained from prawn shell for targeted doxorubicin delivery.

A multifunctional drug carrier with dual targeting (magnetic and folate-receptor) and pH sensitive core-shell hybrid nanomaterial has been developed to carry an anticancer drug doxorubicin.Superparamagnetic iron oxide nanoparticles (IONPs) were used as core of the carrier and cross-linked folate conjugated chitosan (FA-CS) was acted as shell in which doxorubicin was physically entrapped. Transmission electron microscopy (TEM) analysis confirmed the average particle size of IONPs and FA-CS coated IONPs 8.

A WS nanosheet-based nanosensor for the ultrasensitive detection of small molecule-protein interaction via terminal protection of small molecule-linked DNA and Nt.BstNBI-assisted recycling amplification.

Small molecule-protein receptor interactions play vital regulatory roles in molecular diagnostics and therapeutics, chemical genetics, and drug development. However, the rapid, sensitive, low-cost, and selective detection of small molecule-protein receptor interaction remains a challenge. We report herein a new tungsten disulfide (WS) nanosheet-based nanosensor for the ultrasensitive detection of small molecule-protein interaction via terminal protection of small molecule-linked DNA and Nt.

Versatile ligands for high-performance liquid chromatography: An overview of ionic liquid-functionalized stationary phases.

Ionic liquids (ILs), a class of unique substances composed purely by cation and anions, are renowned for their fascinating physical and chemical properties, such as negligible volatility, high dissolution power, high thermal stability, tunable structure and miscibility. They are enjoying ever-growing applications in a great diversity of disciplines. IL-modified silica, transforming the merits of ILs into chromatographic advantages, has endowed the development of high-performance liquid chromatography (HPLC) stationary phase with considerable vitality.

A remarkable enhancement of selectivity towards versatile analytes by a strategically integrated H-bonding site containing phase.

A double β-alanylated L-glutamide-derived organic phase has been newly designed and synthesized in such a way that integrated H-bonding (interaction) sites make it very suitable for the separation of versatile analytes, including shape-constrained isomers, and nonpolar, polar and basic compounds. The β-alanine residues introduced into two long-chain alkyl group moieties provide ordered polar groups through H-bonding among the amide groups.

Design of C18 Organic Phases with Multiple Embedded Polar Groups for Ultraversatile Applications with Ultrahigh Selectivity.

For the first time, we synthesized multiple embedded polar groups (EPGs) containing linear C18 organic phases. The new materials were characterized by elemental analysis, IR spectroscopy, (1)H NMR, diffuse reflectance infrared Fourier transform (DRIFT), solid-state (13)C cross-polarization magic angle spinning (CP/MAS) NMR, suspended-state (1)H NMR, and differential scanning calorimetry (DSC). (29)Si CP/MAS NMR was carried out to investigate the degree of cross-linking of the silane and silane functionality of the modified silica.

Preparation and chromatographic evaluation of new branch-type diamide-embedded octadecyl stationary phase with enhanced shape selectivity.

A novel branch-type diamide-embedded octadecyl stationary phase was prepared by facile amidation. The preparation of this new phase involves the synthesis of new bifunctional silane ligand and surface modification of spherical silica via anchoring of silane coupling agent. The obtained diamide-embedded octadecyl stationary phase demonstrated excellent hydrophobic selectivity, as well as enhanced shape and planarity selectivity in comparison to commercial polymeric and monomeric C18 phases, respectively, as revealed by the systematic investigation into its liquid chromatographic retention of isomeric polycyclic aromatic hydrocarbons.

Highly hydrophilic and nonionic poly(2-vinyloxazoline)-grafted silica: a novel organic phase for high-selectivity hydrophilic interaction chromatography.

A new hydrophilic and nonionic poly(2-vinyloxazoline)-grafted silica (Sil-VOX(n)) phase was synthesized and applied for the separation of nucleosides and nucleobases in hydrophilic interaction chromatography (HILIC). Polymerization and immobilization onto silica were confirmed by using characterization techniques including (1)H NMR spectroscopy, elemental analysis, and diffuse reflectance infrared Fourier transform spectroscopy. The hydrophilicity or wettability of Sil-VOX(n) was observed by measuring the contact angle (59.

Copolymer-grafted silica phase from a cation-anion monomer pair for enhanced separation in reversed-phase liquid chromatography.

This work reports a new imidazolium and L-alanine derived copolymer-grafted silica stationary phase for ready separation of complex isomers using high-performance liquid chromatography (HPLC). For this purpose, 1-allyl-3-octadecylimidazolium bromide ([AyImC18]Br) and N-acryloyl-L-alanine sodium salt ([AAL]Na) ionic liquids (IL) monomers were synthesized. Subsequently, the bromide counteranion was exchanged with the 2-(acrylamido)propanoate organic counteranion by reacting the [AyImC18]Br with excess [AAL]Na in water.

Molecular orientation of gel forming compounds and their effect on molecular-shape selectivity in liquid chromatography.

Double-alkylated glutamic acid and aminoadipic acid derived gel systems (G1 and G2) have been prepared and then grafted onto silica particles. Gel-forming compounds-grafted silica particles (Sil-G1 and Sil-G2) were then applied for the liquid chromatographic separation of shape-constrained isomers of polycyclic aromatic hydrocarbons (PAHs) and tocopherols as stationary phases. G1 and G2 were analyzed before and after immobilization onto silica.

A new imidazolium-embedded C18 stationary phase with enhanced performance in reversed-phase liquid chromatography.

In this paper, a new imidazolium-embedded C(18) stationary phase (SiImC(18)) for reversed-phase high-performance liquid chromatography is described. 1-Allyl-3-octadecylimidazolium bromide ionic liquid compound having a long alkyl chain and reactive groups was newly prepared and grafted onto 3-mercaptopropyltrimethoxysilane-modified silica via a surface-initiated radical-chain transfer addition reaction. The SiImC(18) obtained was characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis, diffuse reflectance infrared Fourier transform, and solid-state (13)C and (29)Si cross-polarization/magic angle spinning nuclear magnetic resonance spectroscopy.

Molecular shape recognition through self-assembled molecular ordering: evaluation with determining architecture and dynamics.

The relationship between molecular gel-forming compound-based double-alkylated L-glutamide-derived functional group-integrated organic phase (Sil-FIP) structure and chromatographic performance is investigated and compared with widely used alkyl phases (C(30), polymeric and monomeric C(18)) as references. The functional group-integrated molecular gel on silica is chemically designed newly in a way that the weak interaction sites are integrated with high orientation and high selectivity can be realized by multiple interactions with the solutes. Its functions can be emphasized by being immobilizable with a terminal carboxyl group and the fact that five amide bonds including β-alanine subunit are integrated per molecule.

Selectivity enhancement for the separation of tocopherols and steroids by integration of highly ordered weak interaction sites along the polymer main chain.

A novel alternating copolymer-based organic phase was synthesized using a new N-substituted maleimide monomer for the development of alternating copolymer-grafted silica for high-performance liquid chromatographic applications. This new monomer (DGMI) was copolymerized with octadecyl acrylate (ODA) from 3-mercaptopropyltrimethoxysilane-grafted silica to produce Sil-poly(ODA-alt-DGMI). The organic phase was characterized by the elemental analysis and the diffuse reflectance infrared Fourier transform spectroscopy.

New poly(ionic liquid)-grafted silica multi-mode stationary phase for anion-exchange/reversed-phase/hydrophilic interaction liquid chromatography.

A new poly(ionic liquid)-grafted silica stationary phase was prepared and characterized. It was then applied for multi-mode chromatographies, including ion-exchange, reversed-phase, and hydrophilic interaction liquid chromatographies for the effective separation of anions, hydrophobic compounds, and small polar molecules, respectively.

Molecular-shape selective high-performance liquid chromatography: stabilization effect of polymer main chain by alternating copolymerization.

This work aims to clarify that stabilization or increased rigidity of polymer main chains as an organic stationary phase can lead the selectivity enhancement in high-performance liquid chromatography (HPLC). For this purpose, the alternating copolymer of octadecyl acrylate (ODA) with a cyclic monomer (N-octadecylmaleimide, OMI) as a rigid segment was synthesized and compared with the ODA homopolymer. Both of the polymer-grafted silicas (Sil-poly(ODA-alt-OMI) and Sil-poly(ODA), respectively) were prepared by radical polymerization on 3-mercaptopropyltrimethoxysilane-modified silica.

New surface-confined ionic liquid stationary phases with enhanced chromatographic selectivity and stability by co-immobilization of polymerizable anion and cation pairs.

Polymerizable ionic liquid monomer pairs were designed and copolymerized on silica as a new strategy to prepare multifunctional hybrid materials in hydrophobic and hydrophilic interaction chromatographies with enhancements of selectivity and stability.

Enhancement of molecular shape selectivity by in situ anion-exchange in poly(octadecylimidazolium) silica column.

This paper demonstrates that in situ anion exchange could be successfully applied as a new method for modifying the surface properties of a poly(octadecylimidazolium)-grafted silica stationary phase to tune and enhance selectivity. Specifically, the original stationary phase was prepared by surface-initiated radical chain-transfer polymerization of 1-vinyl-3-octadecylimidazolium bromide as an ionic liquid monomer; the Br(-) counter anion was then exchanged for methyl orange via an in-column process. As evaluated via the separation of constrained isomers of polycyclic aromatic hydrocarbons (PAHs), the in situ exchange enhanced the molecular shape-selectivity performance.

Molecular-shape selectivity by molecular gel-forming compounds: bioactive and shape-constrained isomers through the integration and orientation of weak interaction sites.

A molecular gel system was assembled on carrier particles and the integrated effect of weak interaction sites enabled highly efficient separation of the bioactive and shape-constrained isomers of tocopherols, β-carotene, and polycyclic aromatic hydrocarbons (PAHs) by multiple interaction mechanisms.