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Recently, CaO‐doped (≤4 mol.%) tetragonal zirconia (CaSZ) ceramic was recommended as a potential alternative to yttria‐stabilized ZrO2 (YSZ). Here, we investigate the limits of starting particle sizes on the stability of tetragonal (t) phase and other associated benefits on measured properties. Synthesized CaSZ powders calcined with different temperatures were used as a mono‐sized or mixed (i.e., two different calcination temperatures) batch fraction for making dense CaSZ ceramic. The mixed‐batch powders were found to be far more efficient in stabilizing the t‐phase in ceramic. Compared to YSZ, CaSZ recorded remarkable enhancement in toughness (up to 8.3 MPa m$\sqrt {\mathrm{m}} $). Contrary to YSZ, CaSZ ceramic demonstrated outstanding thermal stability. [ABSTRACT FROM AUTHOR]

Mixed‐mode chromatography open tubular column has been developed for peptide separation in electrochromatography. A column with 92 cm effective length and 50 μm internal diameter is fabricated internally with a copolymer sheet of restricted thickness. Catalyst facilitated binding of the coupling agent 3,5‐bis (trifluoromethyl) phenyl isocyanate has been carried out at the interior surface of the column. The initiator sodium diethyldithiocarbamate was bound to the coupling agent. A small amount of N‐[2‐(acryloylamino) phenyl] acrylamide was used along with methacrylic acid and styrene in the monomer mixture to induce a little polar character in the stationary phase fabricated inside the column. Twenty‐three peptides have been separated from a chemically digested protein mixture present in cytochrome C in capillary electrochromatography, in addition to the separation of six commercial peptides. We achieved an average plate count of over 1.5 million/m with the column of current study both for the digested protein components and commercial peptides using 70/30% v/v (acetonitrile/20 mM ammonium formate) at pH 6.5. In addition, the column resulted in baseline separation of all the peptides with very good resolution, enhanced peak capacity, and better retention time span. [ABSTRACT FROM AUTHOR]

A particle‐based stationary phase has been prepared for the separation of five synthetic peptides and a mixture containing tryptic digest of cytochrome C in liquid chromatography. Particles originating from silica monolith were differentially sedimented to obtain 1–2 μm particles. A stationary phase was achieved by the coating of poly(styrene‐methacrylic acid‐N‐phenylacrylamide) copolymer onto the particles via reversible addition‐fragmentation chain transfer polymerization reaction. Stainless steel column (30 cm long and 1 mm internal diameter) was packed with stationary phase. Very high separation efficiency (ca. 351 000 plates/m) was achieved for five commercial peptides with a percent relative standard deviation of less than 1%. Protocol for the synthesis and modification of silica monolith particles has been well optimized with a good reproducibility both in particle and pore size. The column resolved about 21 peptide components from a mixture containing tryptic digest of cytochrome C, under the elution conditions of acetonitrile/15 mM ammonium format (65/35 v/v%) with a flow rate of 28 μL/min. [ABSTRACT FROM AUTHOR]

The article explores on the clinical diagnostics of disease mechanisms and biomarker discovery of proteomic samples. It examines the separation of peptides in the open tubular capillary electrochromatography (OT-CEC) columns. It also cites the formulations of the polymerization mixtures in the polar monomer.

A silica capillary of 50 μm internal diameter and 500 mm length (416 mm effective length) was chemically modified with 4-(trifluoromethoxy) phenyl isocyanate in the presence of dibutyl tin dichloride as catalyst. Sodium diethyl dithiocarbamate was reacted with the terminal halogen of the bound ligand to incorporate the initiator moiety, and in situ polymerization was performed using a monomer mixture of styrene, N-phenylacrylamide, and methacrylic acid. The resultant open tubular capillary column immobilized with the copolymer layer was used for the separation of tryptic digest of cytochrome C in capillary electrochromatography. The sample was well eluted and separated into many components. The elution patterns of tryptic digest of cytochrome C were studied with respect to pH and water content in the mobile phase. This preliminary study demonstrates that open tubular capillary electrochromatography columns with a modified copolymer layer composed of proper nonpolar and polar units fabricated by reversible addition-fragmentation transfer polymerization can be useful as separation media for proteomic analysis. [ABSTRACT FROM AUTHOR]

A ligand with a terminal halogen (4-chloromethylphenyl isocyanate) was chemically bound on the inner surface of pretreated silica capillary with 50 μm internal diameter and 58 cm total and 50 cm effective length in the presence of dibutyl tin dichloride as a catalyst through isocyanate-hydroxyl reaction. Attachment of initiator (sodium diethyl dithiocarbamate) to the bound ligand was carried out and followed by in situ polymerization. Reversible addition-fragmentation chain transfer polymerization was used for the immobilization of N-phenylacrylamide-styrene copolymer on the inner surface of capillary column. The resultant open tubular column showed excellent separation performance for derivatized saccharide isomers in capillary electrochromatography. d-Glucose was separated into α- and β-anomers while five structural isomers were separated for derivatized maltotriose with separation efficiency above one million theoretical plates per meter. The effects of pH and acetonitrile composition on the electrochromatographic performance of the derivatized saccharides were studied and the optimized elution condition was found to be 90:10 v/v% acetonitrile/30 mM sodium acetate at pH 6.6. UV absorption at 214 nm was used as detection mode in open tubular capillary electrochromatography separations. [ABSTRACT FROM AUTHOR]

Ground porous silica monolith particles with an average particle size of 2.34 μm and large pores (363 Å) exhibiting excellent chromatographic performance have been synthesized on a relatively large scale by a sophisticated sol-gel procedure. The particle size distribution was rather broad, and the d(0.1)/ d(0.9) ratio was 0.14. The resultant silica monolith particles were chemically modified with chlorodimethyloctadecylsilane and end-capped with a mixture of hexamethyldisilazane and chlorotrimethylsilane. Very good separation efficiency (185 000/m) and chromatographic resolution were achieved when the C18-bound phase was evaluated for a test mixture of five benzene derivatives after packing in a stainless-steel column (1.0 mm × 150 mm). The optimized elution conditions were found to be 70:30 v/v acetonitrile/water with 0.1% trifluoroacetic acid at a flow rate of 25 μL/min. The column was also evaluated for fast analysis at a flow rate of 100 μL/min, and all the five analytes were eluted within 3.5 min with reasonable efficiency (ca. 60 000/m) and resolution. The strategy of using particles with reduced particle size and large pores (363 Å) combined with C18 modification in addition to partial-monolithic architecture has resulted in a useful stationary phase (C18-bound silica monolith particles) of low production cost showing excellent chromatographic performance. [ABSTRACT FROM AUTHOR]

The article discussed a study which focused on the synthesis of silica monolith particles. Topics discussed include chemical modification of the silica monolith particles using C-18 alkyl ligand, particle size distribution of the silica monolith particles, and analysis of the molecules using high performance liquid chromatography (HPLC).

Molecular imprinted polymer is an artificial receptor made by imprinting molecules of a template in a polymer matrix followed by removing the template molecules via thorough washing to give the permanent template grooves. They show favored affinity to the template molecule compared to other molecules, and this property is the basic driving force for such diverse application of this techniques. Such techniques have been increasingly employed in a wide scope of applications such as chromatography, sample pretreatment, purification, catalysts, sensors, and drug delivery, etc., mostly in bioanalytical areas. A major part of them is related to development of new stationary phases and their application in chromatography and sample pretreatment. Embodiments of molecular imprinted polymer materials have been carried out in a variety of forms such as irregularly ground particles, regular spherical particles, nanoparticles, monoliths in a stainless steel or capillary column, open tubular layers in capillaries, surface attached thin layers, membranes, and composites, etc. There have been numerous review articles on molecular imprinted polymer issues. In this special review, the reviews in recent ca. 10 years will be categorized into several subgroups according to specified topics in separation science, and each review in each subgroup will be introduced in the order of date with brief summaries and comments on new developments and different scopes of prospects. Brief summaries of each categories and conclusive future perspectives are also given. [ABSTRACT FROM AUTHOR]