Synthesis of covalently bonded cellulose derivative chiral stationary phases with a bifunctional reagent of 3-(triethoxysilyl)propyl isocyanate

A bifunctional reagent of 3-(triethoxysilyl)propyl isocyanate (TEPI) was initially adopted as a spacer reagent to prepare the bonded types of chiral stationary phases (CSPs) with cellulose derivatives. The silica-based CSPs were chemically prepared with non-regioselective and regioselective approaches and their chiral resolving capabilities were evaluated in terms of HPLC resolution of test enantiomers. It was observed that the chiral recognition capabilities of the non-regioselectively prepared CSPs were influenced by the amount of TEPI used. And also, the regioselectively prepared CSP generally showed a slightly higher resolution power than the non-regioselectively prepared CSP, while the non-regioselective procedures were highly advantageous to rapid preparation. In addition, chiral recognition of the prepared CSPs was affected by the properties of the used silica matrices. (C) 2003 Elsevier B.V. All rights reserved.

Determination of 1-phenyl-3-methyl-5-pyrazolone-labeled carbohydrates by liquid chromatography and micellar electrokinetic chromatography

In this paper, the method for the derivatization of carbohydrates with 1-phenyl-3-methyl-5-pyrazolone (PMP) was simplified. One-third of the derivatization time was saved. Five monosaccharide derivatives have been well separated by MEKC and HPLC under optimized conditions. Good reproducibility could be obtained with relative standard deviation (RSD) values of the migration times within 5.0 and 2.3%, respectively. Furthermore, the developed methods have been successfully applied to the analysis of carbohydrates in Aloe powder and food. These methods are quite useful for routine analysis of monosaccharides and oligosaccharides in real samples. (C) 2003 Elsevier B.V. All rights reserved.

2-D and 3-D processing and interpretation of multi-fold ground penetrating radar data:a case history from an archaeological site

A 2.5-D and 3-D multi-fold GPR survey was carried out in the Archaeological Park of Aquileia (northern Italy). The primary objective of the study was the identification of targets of potential archaeological interest in an area designated by local archaeological authorities. The second geophysical objective was to test 2-D and 3-D multi-fold methods and to study localised targets of unknown shape and dimensions in hostile soil conditions. Several portions of the acquisition grid were processed in common offset (CO), common shot (CSG) and common mid point (CMP) geometry. An 8×8 m area was studied with orthogonal CMPs thus achieving a 3-D subsurface coverage with azimuthal range limited to two normal components. Coherent noise components were identified in the pre-stack domain and removed by means of FK filtering of CMP records. Stack velocities were obtained from conventional velocity analysis and azimuthal velocity analysis of 3-D pre-stack gathers. Two major discontinuities were identified in the area of study. The deeper one most probably coincides with the paleosol at the base of the layer associated with activities of man in the area in the last 2500 years. This interpretation is in agreement with the results obtained from nearby cores and excavations. The shallow discontinuity is observed in a part of the investigated area and it shows local interruptions with a linear distribution on the grid. Such interruptions may correspond to buried targets of archaeological interest. The prominent enhancement of the subsurface images obtained by means of multi-fold techniques, compared with the relatively poor quality of the conventional single-fold georadar sections, indicates that multi-fold methods are well suited for the application to high resolution studies in archaeology.