A new heterostructured material is synthesized with lamellar arrangements in nanoscale precision through an innovative synthetic approach. The self-assembled Ni-based cyano-bridged coordination polymer flakes (Ni-CP) and graphene oxide (GO) nanosheets with a layered morphology (Ni-CP/GO) are used as precursors for the synthesis of multicomponent hybrid materials. Annealing of Ni-CP/GO in nitrogen at 450 °C allows the formation of Ni C/rGO nanocomposites.
View Article and Find Full Text PDFCyclodextrin-modified micellar ultra pressure liquid chromatography (CD-MUPLC) was firstly developed and directly applied to the simultaneous determination of water-soluble vitamins thiamine hydrochloride (VB1), pyridoxine hydrochloride (VB6) and ascorbic acid (VC) in milk samples. A hybrid isocratic mobile phase consisting of β-cyclodextrin (β-CD, 5.0 mmol L-1) and cetyltrimethylammonium bromide (CTAB, 0.
View Article and Find Full Text PDFA rapid and sensitive ultrasound-assisted temperature-controlled ionic liquid (IL) dispersive liquid-phase microextraction (UTILDLPME) combined with reversed-phase liquid chromatography-ultraviolet (RPLC-UV) was developed for the determination of five organophosphorus pesticides (OPPs; azinphos-methyl, chloropyriphos, parathion-methyl, diazinon, and phosalone) in water samples. Parameters including IL type, IL volume, ionic strength, sonication time, heating/cooling temperature, centrifugal time, and speed were investigated. The extraction procedure was induced by the formation of cloudy solution, which was composed of 75 μL of 1-butyl-3-methylimidazolium hexafluorophosphate ([C4MIM]PF ) dispersed entirely into 5 mL sample solution with the assistance of ultrasound for 3 min and temperature at 40°C.
View Article and Find Full Text PDFThe popularity of ionic liquids (ILs) has grown during the last decade in enhancing the sensitivity of CE through different off-line or on-line sample preconcentration techniques. Water-insoluble ILs were commonly used in IL-based liquid phase microextraction, in all its variants, as off-line sample preconcentration techniques combined with CE. Water-soluble ILs were rarely used in IL-based aqueous two phase system (IL-ATPS) as an off-line sample preconcentration approach combined with CE in spite of IL-ATPS predicted features such as more compatibility with CE sample injection due to its relatively low viscosity and more compatibility with CE running buffers avoid, in some cases, anion exchange precipitation.
View Article and Find Full Text PDFRecently, ionic liquids (ILs) are finding ever broader scope within pharmaceutical and bioanalytical applications. In the current work, ACE binding measurements of tryptophan (Try)-HSA, chlorambucil (CHL)-HSA, and dacarbazine (DTIC)-HSA complexes were estimated in the absence or presence of several short chain imidazolium ILs within the range of concentrations of 10.0-1000.
View Article and Find Full Text PDFTo facilitate the implementation of affinity capillary electrophoresis into routine binding screening studies of proteins with metal ions, method acceleration, transfer and precision improvement were investigated. Affinity capillary electrophoresis was accelerated by using shorter capillaries, employing lower sample concentrations and smaller injection volumes. Intra- and inter-instrument method transfers were investigated considering the temperature setting of the capillary cooling system.
View Article and Find Full Text PDFDespite its importance and all the considerable efforts made, the progress in drug discovery is limited. One main reason for this is the partly questionable data quality. Models relating biological activity and structures and in silico predictions rely on precisely and accurately measured binding data.
View Article and Find Full Text PDFThe present review covers recent advances and important applications of affinity capillary electrophoresis (ACE). It provides an overview about various ACE types, including ACE-MS, the multiple injection mode, the use of microchips and field-amplified sample injection-ACE. The most common scenarios of the studied affinity interactions are protein-drug, protein-metal ion, protein-protein, protein-DNA, protein-carbohydrate, carbohydrate-drug, peptide-peptide, DNA-drug and antigen-antibody.
View Article and Find Full Text PDFJ Chromatogr B Analyt Technol Biomed Life Sci
October 2014
Determination of tea catechins in human plasma might provide a means of better evaluation of their benefits. The main difficulty in their analysis is the low catechins concentrations in plasma and their susceptible to oxidation during sample pretreatment. In the current work, a sweeping-micellar electrokinetic chromatography (sweeping-MEKC) by long alkyl chain ionic liquid was investigated for the simultaneous determination of seven principal naturally-occurring tea catechins in human plasma under acidic conditions after the intake of green tea beverage.
View Article and Find Full Text PDFResearch on sodium batteries has made a comeback because of concern regarding the limited resources and cost of lithium for Li-ion batteries. From the standpoint of electrochemistry and economics, Mn- or Fe-based layered transition metal oxides should be the most suitable cathode candidates for affordable sodium batteries. Herein, this paper reports a novel cathode material, layered Na1+x(Fey/2Niy/2Mn1-y)1-xO2 (x = 0.
View Article and Find Full Text PDFTransition metal dichalcogenides (TMD), analogue of graphene, could form various dimensionalities. Similar to carbon, one-dimensional (1D) nanotube of TMD materials has wide application in hydrogen storage, Li-ion batteries, and supercapacitors due to their unique structure and properties. Here we demonstrate the feasibility of tungsten disulfide nanotubes (WS2-NTs)/graphene (GS) sandwich-type architecture as anode for lithium-ion batteries for the first time.
View Article and Find Full Text PDFIn this study, size-exclusion chromatography and high-resolution atomic absorption spectrometry methods have been developed and evaluated to test the stability of proteins during sample pretreatment. This especially includes different storage conditions but also adsorption before or even during the chromatographic process. For the development of the size exclusion method, a Biosep S3000 5 μm column was used for investigating a series of representative model proteins, namely bovine serum albumin, ovalbumin, monoclonal immunoglobulin G antibody, and myoglobin.
View Article and Find Full Text PDFThe binding of physiologically anionic species or negatively charged drug molecules to proteins is of great importance in biochemistry and medicine. Since affinity capillary electrophoresis (ACE) has already proven to be a suitable analytical tool to study the influence of ions on proteins, this technique was applied here for comprehensively studying the influence of various anions on proteins of BSA, β-lactoglobulin, ovalbumin, myoglobin, and lysozyme. The analysis was performed using different selected anions of succinate, glutamate, phosphate, acetate, nitrate, iodide, thiocyanate, and pharmaceuticals (salicylic acid, aspirin, and ibuprofen) that exist in the anionic form at physiological pH 7.
View Article and Find Full Text PDFSince the introduction about 30 years ago, CE techniques have gained a significant impact in pharmaceutical analysis. The present review covers recent advances and applications of CE for the analysis of pharmaceuticals. Both small molecules and biomolecules such as proteins are considered.
View Article and Find Full Text PDFAcrylamide in food has drawn worldwide attention since 2002 due to its neurotoxic and carcinogenic effects. These influences brought out the dual polar and non-polar characters of acrylamide as they enabled it to dissolve in aqueous blood medium or penetrate the non-polar plasma membrane. In the current work, a simple HPLC/UV system was used to reveal that the penetration of acrylamide in non-polar phase was stronger than its dissolution in polar phase.
View Article and Find Full Text PDFThe current work presents analytical procedures for simultaneous determination of tarabine PFS and adriblastina by micellar electrokinetic chromatography (MEKC) and liquid chromatography (LC). For MEKC analysis, separations and identifications were accomplished using uncoated fused-silica capillary with hydrodynamic injections in the presence of 50mM borate/phophate pH 8.7 and 100mM SDS.
View Article and Find Full Text PDFA simple and reliable analytical electrophoretic method using chiral capillary electrophoresis (CCE) with a high-sensitivity cell of special design has been established for simultaneous determination of (+)-catechin (C) and (-)-epicatechin (EC) in aqueous and human plasma media. The application of a capillary with high-sensitivity cell has led to an improvement of 10-fold and 5-fold time-corrected peak area over a standard cell and a capillary with bubble cell, respectively. Analysis has involved the electrophoretic separation of C and EC in less than 4.
View Article and Find Full Text PDFChiral CE was successfully applied to the separation and quantification of catechin, epicatechin and ascorbic acid in some commercial drinks and human urine. Analysis involved the separation of analytes in less than 5.0 min at 240 nm with an untreated fused-silica capillary under hydrodynamic injection mode.
View Article and Find Full Text PDF(+)-Catechin (CAT) was considered as a polyphenolic compound abundantly contained in plants. It exerts protective effect against cancer, inflammatory and cardiovascular diseases. These protective effects are mainly attributed to its antioxidative activity by scavenging free radicals.
View Article and Find Full Text PDFA cyclodextrin-modified micellar electrokinetic chromatographic (CD-MEKC) method for the determination of the most important potential impurities of methotrexate (MTX): 2,4-diamino-6-(hydroxymethyl)pteridine, aminopterine hydrate, 4-[N-(2-amino-4-hydroxy-6-pteridinylmethyl)-N-methylamino] benzoic acid, 4-[N-(2,4-diamino-6-pteridinylmethyl)-N-methylamino] benzoic acid, and the distomer D-MTX is presented. The MEKC separation of these compounds was optimized by applying a step-by-step approach. The addition of beta-CD to a conventional MEKC system, based on sodium dodecyl sulfate (SDS) as surfactant, showed to be essential for the enantioresolution of racemic MTX as well as for the separation of the achiral impurities.
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