Reversed capillary electrochromatography: Investigation of peak symmetry for eluting curves of solutes

The transport processes of components in capillary electrochromatographic column was investigated based on the basic model of relaxation theory. A principal transport equation of chromatographic relaxation theory was established and mathematical expressions for eluting curves were obtained under the situations of both capillary electrophoresis and chromatography. Characteristics of peak symmetry and its effecting factors are discussed. Tailing peaks, symmetrical peaks and fronting peaks would be observed simultaneously, which was further proved with reversed capillary electrochromatographic experiments.

Separation of enantiomers by nanoliquid chromatography and capillary electrochromatography using a bonded cellulose trisphenylcarbamate stationary phase

A cellulose trisphenylcarbamate-bonded chiral stationary phase was applied to nano-liquid chromatography (nano-LC) and capillary electrochromatography (CEC) with nonaqueous and aqueous solutions as the mobile phases. Several chiral compounds were successfully resolved on the prepared phase by nano-LC. The applicability of nonaqueous CEC on a cellulose derivative stationary phase was investigated with the organic solvents methanol, hexane, 2-propanol, and tetrahydrofuran (THF) containing acetic acid, as well as triethylamine as the mobile phases. Enantiomers of warfarin and praziquantel were baseline-resolved with plate numbers of 82 300 and 38 800 plates/m, respectively, for the first eluting enantiomer. The influence of applied voltage, concentration of nonpolar solvent, apparent pH, and buffer concentration in the mobile phase on the electroosmotic flow (EOF) and the mobility of the enantiomers was evaluated. Enantioseparations of traps-stilbene oxide and praziquantel were also achieved in aqueous CEC with plate numbers of 111 100 and 107 400 plates/m, respectively, for the first eluting enantiomer. A comparison between nonaqueous CEC and aqueous CEC based on a cellulose trisphenylcarbamate stationary phase was discussed. Pressure-assisted CEC was examined for the chiral separation of praziquantel and faster analysis with high enantioselectivity was acquired with the proper pressurization of the inlet vial.

Biodegradation of poly(L-lactide-co-glycolide) tube stents in bile

The objective of this study was to evaluate degradation behavior and the feasibility of biodegradable polymeric stents in common bile duct (CBD) repair and reconstruction. Various molar ratios of lactide (LA) and glycolide (GA) in poly(L-lactide-co-glycolide) (PLGA) were synthesized and processed into a circular tubing of similar to 10.0 mm outer diameter and a wall thickness of about 2.0 mm.

Feasibility of biodegradable PLGA common bile duct stents: An in vitro and in vivo study

The current study investigates the feasibility of using a biodegradable polymeric stent in common bile duct (CBD) repair and reconstruction. Here, poly(l-lactide-co-glycolide) (PLGA, molar ratio LA/GA = 80/20) was processed into a circular tube- and dumbbell-shaped specimens to determine the in vitro degradation behavior in bile. The morphology, weight loss, and molecular weight changes were then investigated in conjunction with evaluations of the mechanical properties of the specimen. Circular tube-shaped PLGA stents with X-ray opacity were subsequently used in common bile duct exploration (CBDE) and primary suturing in canine models. Next, X-ray images of CBD stents in vivo were compared and levels of serum liver enzymes and a histological analysis were conducted after stent transplantation. The results showed that the PLGA stents exhibited the required biomedical properties and spontaneously disappeared from CBDs in 4-5 weeks. The degradation period and function match the requirements in repair and reconstruction of CBDs to support the duct, guide bile drainage, and reduce T-tube-related complications.

Hydrodynamic radius characterization of a vinyl-type polynorbornene by size-exclusion chromatography with a static and dynamic laser light scattering detector

Both absolute molecular weight and molecular sizes (radius of gyration and hydrodynamic radius) of a vinyl-type polynorbornene eluting from size-exclusion chromatography columns were determined by combined with a static and dynamic laser light scattering detector. The hydrodynamic radius of polymer fraction eluting from size-exclusion chromatography columns was obtained from dynamic laser light scattering measurements at only a single angle of 900 by introducing a correction factor. According to the scaling relationship between molecular sizes and molecular weight and the ratio between radius of gyration and hydrodynamic radius, the vinyl-type polynorbornene took a random coil conformation in 1,2,4-trichlorobenzene at 150 degreesC.

Investigation of the effect of branched structure on the performances of the copolymers synthesized from ethylene and alpha-olefin with rac-Et(Ind)(2)ZrCl2/MMAO catalyst system

The branched copolymers prepared from ethylene and alpha-olefins using rac-Et(Ind)(2)ZrCl2/MMAO catalyst system were studied. Both the absolute molecular weight ((M) over bar (W)) and the molecular size (radius of glyration, R-g) of the polymers eluting from gel permeation chromatography (GPC) columns were obtained simultaneously via a high temperature GPC coupled with a two-angle laser light scattering (TALLS) detector. The branched structures and performances of the copolymers display approximate molecular weight and molecular sizes were investigated. Wide angle X-ray diffraction analyses indicate that 16-carbon side branch could co-crystallize effectively with backbone chain at low alpha-olefin incorporation. The melt behaviors of the copolymers were studied by dynamic rheological measurements. Both branch length and comonomer content affect considerably the loss modulus, storage modulus and complex viscosity of the copolymers. The relationship between the dynamic-mechanical behavior and the comonomer content of the copolymers was also examined by dynamic-mechanical experiments.

Determination of molecular weight and molecular sizes of polymers by high temperature gel permeation chromatography with a static and dynamic laser light scattering detector

Flow-mode static and dynamic laser light scattering (SLS/DLS) studies of polymers, including polystyrene, polyethylene, polypropylene and poly(dimethylsiloxane) (PDMS), in 1,2,4-trichlorobenzene (TCB) at 150 degreesC were performed on a high temperature gel permeation chromatography (GPC) coupled with a SLS/DLS detector. Both absolute molecular weight (M) and molecular sizes (radius of gyration, R-g and hydrodynamic radius, R-h) of polymers eluting from the GPC columns were obtained simultaneously. The conformation of different polymers in TCB at 150 degreesC were discussed according to the scaling relationships between R-g, R-h and M and the rho-ratio (p = R-g/R-h). Flow-mode DLS results of PDMS were verified by batch-mode DLS study of the same sample. The presented technique was proved to be a convenient and quick method to study the shape and conformation of polymers in solution at high temperature. However, the flow-mode DLS was only applicable for high molecular weight polymers with a higher refractive index increment such as PDMS.

Column switching-back flushing technique for the analysis of aromatic compounds in gasoline

A simple method, based on the technique of capillary column switching-back flushing, has been developed for the detailed analysis of aromatic compounds in gasoline. The sample was first separated on a 30-m long OV-2330 polar precolumn and then backflushed onto a nonpolar analytical column. The early eluting components from the precolumn and the components of interest (aromatic compounds plus heavier compounds) eluting from the analytical column are all directed to the same flame ionization detection system through a T piece, which permits the quantitative analysis of aromatic hydrocarbons in gasoline by a normalization method using correcting factors. The switching time window of the method is +/-5 s, resulting in easier operation and higher reliability. The reproducibility of the quantitative analysis was less than or equal to3% RSD for real gasoline samples. (C) 2002 Elsevier Science B.V. All rights reserved.

Development and application of a sol-gel immunosorbent-based method for the determination of isoproturon in surface water

An immunosorbent was fabricated by encapsulation Of monoclonal anti-isoproturon antibodies in sol-gel matrix. The immunosorbent-based loading, rinsing and eluting processes were optimized. Based on these optimizations, the sol-gel immunosorbent (SG-IS) selectively extracted isoproturon from an artificial mixture of 68 pesticides. In addition to this high selectivity, the SG-IS proved to be reusable. The SG-IS was combined with liquid chromatography-tandem mass spectrometry (LC-MS-MS) to determine isoproturon in surface water, and the linear range was up to 2.2 mu g/l with correlation coefficient higher than 0.99 and relative standard deviation (RSD) lower than 5% (n = 8). The limit of quantitation (LOQ) for 25-ml surface water sample was 5 ng/l. (c) 2006 Elsevier B.V. All rights reserved.