Determination of the chemical structure of potential organic impurities occurring in the drug substance opipramol.

The tricyclic antipsychotic and antidepressant drug opipramol (opipramole) was examined with regard to the chemical structure of its organic impurities. Impurities were isolated from the technical product by chromatographic methods and their chemical structures were established by 1H NMR, MS and FTIR and further confirmed by comparison with commercially available products or with products obtained by independent synthesis, and in one case additionally by X-ray structure analysis.

Metal-coated fused silica fibers as a support for immobilized compounds yielding a volatile analyte (C2H4).

This paper presents the results of investigations of chemically modified fibers comprising an immobilized compound that yields ethene as the analyte in generated standard gaseous mixtures. Prior to chemical modification, the fibers were coated with a thin aluminum layer to improve their mechanical strength. Commercially available Al-coated fibers were used in this work. During thermal decomposition of the immobilized compound, reproducible quantities of the analyte per unit fiber length were obtained for all the investigated fibers (fiber diameter (microm)/outside diameter (microm) of the Al-coated fiber=110/146, 220/300, and 660/830), amounting to 0.685+/-0.032, 0.8300+/-0.0081, and 1.092+/-0.010 ng cm(-1), respectively. The proposed procedure can be used successfully for the generation of measured component of matrix-free reference materials.

New procedure of silica gel surface modification preparation of gaseous standard mixtures for calibration purposes.

The new type of silica gel surface modification with using the trimethylamine as a reagent is described. The samples of chemically modified silica gel have been used for generation of gaseous standard mixtures (methyl chloride as a measurand) using the technique of thermal decomposition of the surface compound. The main aim of the research was to check the suitability of the new type of silica gel surface modification for obtaining methyl chloride as a measurand of gaseous standard mixture. The gaseous standard mixture obtained with using this technique was used for calibration of a thermal desorber-gas chromatography-flame ionization detector (TD-GC-FID) system. The homogeneity of coverage of silica gel surface with the immobilized compound has been evaluated. The full uncertainty budget of determination of liberated amount of methyl chloride has been calculated. The average amount of methyl chloride liberated from the unit sample of chemically modified silica gel is 3.59 +/- 0.13 mg g(-1). The influence of the modification way on the amount of liberated analyte has also been determined.

Use of porous glass and silica gel as support media of a surface compound for generation of analytes in gaseous standard mixtures. New method for the determination of the amount of analyte generated.

The paper presents a new method for the determination of a volatile component of a gaseous standard mixture obtained by thermal decomposition of a suitable surface compound. The amount of the analyte generated (under given conditions of thermal decomposition) per unit of mass of the chemically modified material has been determined exclusively on the basis of measuring generation time. Therefore, the total error of the determination of the amount of a standard compound depends solely on the respective errors of weighing the material and measuring its decomposition time (both being direct measurements). This new method permits obtaining a few measuring points on the basis of a single sample of the material with chemically modified surface.