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Biomedical subjects

W Baeyens

Publications and source records attributed to W Baeyens.

At least 37 records · Page 2Linked to original sources

Enantiomeric separation of amide derivatives of some 2-arylpropionic acids by HPLC on a cellulose-based chiral stationary phase.

A reversed phase high-performance liquid chromatographic method has been developed for the determination of the R- and S-enantiomers of ibuprofen, flurbiprofen, ketoprofen and tiaprofenic acid. Separation has been achieved using a tris(4-methylbenzoate)cellulose phase after derivatization into their amides. Flurbiprofen could also be partially resolved into its enantiomers without prior derivatization.

Amides↗

Separation of 2-arylpropionic acids on a cellulose based chiral stationary phase by RP-HPLC.

The enantiomers of eight 2-arylpropionic acids, a group of chiral non steroidal antiinflammatory drugs, were resolved as their benzylamide derivatives on a high-performance liquid chromatographic chiral stationary phase consisting of a covalently bound tris (4-methylbenzoate) cellulose layer on silica gel. The column was used under reversed-phase conditions using methanol as the main mobile phase component, with a perchlorate buffer pH 2.0. A compromise for derivatization with a water soluble carbodiimide and 1-hydroxybenzotriazole of a group of eight analytes was obtained. The derivatives were identified by IR- and MS-spectroscopy.

Amides↗

Sensitive spectrofluorimetric determination of tetracycline residues in bovine milk.

A novel, sensitive, high-performance liquid chromatographic method for the residue determination of tetracyclines in bovine milk has been developed. Clean-up of the sample extracts is performed with metal chelate affinity chromatography. Detection is based upon the measurement of fluorescence induced by complexation of tetracyclines with the zirconium cation, which is added post-column to the high-performance liquid chromatographic eluate. The method has been validated for oxytetracycline, tetracycline and chlortetracycline. Calibration curves using 'blank' milk fortified at the 10-200 ng ml-1 level showed good linear correlation. Accuracy was measured at the 100 ng ml-1 level and was found to be within acceptable limits using a t-test (alpha = 0.05). At this level both within- and between-day precision, as measured by relative standard deviation (S(r)), were less than 16% for oxytetracycline and chlortetracycline, and less than 20% for tetracycline. The most striking advantages of the proposed method, over previously reported methods, are the higher sensitivity and specificity achieved. Using a signal-to-noise ratio of 4:1, the detection limits of the assay were 1 ng ml-1 for oxytetracycline, 2 ng ml-1 for tetracycline and 4 ng ml-1 for chlortetracycline.

Animals↗

Analysis of pilocarpine and its trans epimer, isopilocarpine, by capillary electrophoresis.

Capillary zone electrophoresis was used for the separation of pilocarpine from its epimer, isopilocarpine, using coated fused-silica capillaries of 20 cm x 25 microm I.D., 8 kV running voltage, migration buffer of 0.1 M sodium dihydrogenphosphate pH 8, detection at 217 nm and injection by electromigration. Injections of aqueous, acid and basic solutions were compared. Linearity of the signal for pilocarpine hydrochloride up to 200 microg ml(-1) in 0.05 M hydrochloric acid was obtained, using naphazoline nitrate as internal standard. Optimization of migration buffer pH using coated silica capillaries of 50 cm x 50 microm I.D. showed that at pH 6.9 pilocarpine can be separated from ++isopilocarpine. Inclusion of beta-cyclodextrin in the buffer allows full baseline separation of both epimers. The method was applied to the analysis of a commercial ophthalmic pilocarpine solution.

Buffers↗

Evaluation of gas chromatographic columns for the determination of methylmercury in aqueous head space extracts from biological samples.

Several gas chromatographic columns were evaluated for the determination of methylmercury in aqueous solution. The goal of the study was to further decrease the detection limit of the recently developed method of head space gas chromatography with microwave-induced plasma detection (HS-GC-MIP) for the determination of methylmercury in biological samples. The columns were first evaluated using gas chromatography with electron-capture detection (ECD). At the same time, the column efficiencies for the determination of ethyl- and phenylmercury were also studied. Of the packed columns the stationary phase used previously in HS-GC-MIP, AT-1000, yielded the best results. Better results were obtained with two wide-bore thick-film fused-silica open tubular (FSOT) columns, one of which was suitable for aqueous injections (Superox-FA) and the other for benzene or toluene (RSL-300). With these FSOT columns, absolute detection limits at the sub-picogram level were reached. A new HS-GC-MIP system was then constructed, which was adapted for the use of FSOT columns. As more sensitive measurements were obtained with a Superox-FA FSOT column than with an AT-1000 packed column using the GC-ECD system in the first part of this study, the FSOT column was evaluated in this HS-GC-MIP system for the determination of methylmercury in real tissue samples. It was demonstrated that the use of an FSOT column gives only a small decrease in the detection limit compared with a packed column; reconditioning of the FSOT column is, however, a disadvantage in routine measurements.

Chromatography, Gas↗

Chromatographic isolation and mass spectrometric identification of a base-induced mebendazole fluorophor.

Sodium hydroxide treatment of the benzoylbenzimidazole anthelmintics mebendazole and flubendazole produces yellow solutions that possess practically no fluorescence characteristics under various conditions. However, when spotting the alkaline solutions on filter paper and examining the spots under U.V., strong bluish-white fluorescence is obtained. When pouring liquid nitrogen over the spots, a very intense bluish-white fluorescence followed by a long-lasting greenish phosphorescence is observed. These luminescence phenomena allow visualization of 1 ng of mebendazole and of 5 ng of flubendazole per spot. A preparative separation by means of column liquid chromatography was worked out for the isolation of the fluorophor in case of mebendazole. Combined spectroscopic methods indicated the formation of a primary amine function in position 2 of the imidazole nucleus by hydrolytic cleavage of the -NH-CO-bond. A discussion on the mechanism of fluorescence is given.

Mebendazole↗

Fluorimetric analysis of mebendazole and flubendazole with hydrogen peroxide.

Analytically useful fluorescence was obtained from mebendazole and flubendazole after reaction with hydrogen peroxide in alkaline solution. The fluorescence produced (lambda(ex) = 300 nm; lambda(em) = 360 nm) is stable and concentrations of 0.1 mug ml(-1) can be determined. The method has been applied to the analysis of some commercially available anthelmintic preparations.

Journal Article↗

On the altered nucleocytoplasmic transport "in vitro" of rapidly labelled RNA, in the presence of cytosol or serum from tumor-bearing rats.

Enhanced nucleocytoplasmic RNA transport has been demonstrated by incubating normal rat liver nuclei in presence of cytosols originating from the poorly differentiated, fast-growing hepatoma HW-165, in the linear phase of tumor growth. The effect of hepatoma HW-165 cytosol was reduced or suppressed in presence of small amounts of normal liver cytosol: on the other hand, several polypeptides of molecular weight 20,000 to 40,000 daltons were hardly detectable in hepatoma HW-165 cytosol, both arguments indicating that potentially regulatory proteins should be absent or present in reduced concentration in hepatoma HW-165 cytosol. No modification of RNA release was observed in presence of cytosols originating from the thymus of RNA virus (BL/F)-infected rats, whatever be the time after inoculation. Attempts were made to use the nuclear restriction assay, supplemented with plasma or serum of various origins, as a biochemical marker of neoplasia. In a first series of assays, including 80 cancer patients and 12 healthy controls, the RNA transport activity was stimulated by the serum of patients bearing various tumors (lung cancer, cancer of the respiratory tract, uterine cervix...), except in a few cases of mammary carcinoma, where values equivalent to or lower than the controls were obtained.

Animals↗

Thyroid influence on the growth of hepatoma HW-165 in Wistar rats.

The development of a fast-growing hepatoma (HW-165) in normal euthyroid Wistar rats, was shown to be stimulated by daily injection of a dose of triiodo-L-thyronine (T3) as low as 1.5 microgram/100 g body weight. Administered to thyroidectomized rats, T3 completely restored the frequency of tumor initiation and accelerated the growth of the hepatoma, which had been considerably slowed down in hypothyroid rats. Contrary to other investigators, working on fast-growing Morris hepatomas, we did not observe any significant increase in the T3 level in the serum of hepatoma HW-165-bearing rats. Similarly, the tetra-iodo-L-thyronine (T4) levels were of the same order of magnitude in the blood of both normal and tumor host animals. The mitotic activity was reduced in hepatomas transplanted in hypothyroid rats and increased in tumors of T3-treated animals. These results support the assertion of Short (20) suggesting a relationship between the mitogenic effects of iodothyronines on the normal hepatocyte and on transplanted tumors of hepatic origin.

Animals↗

Fluorescence properties of glafenine.

The fluorescence properties of glafenine are partly caused by the anthranilic acid nucleus of the molecule. Correlations are made between fluorescence capacities and UV absorbance. Analytical determinations can be carried out in different solvents, e.g., ether, benzene, and ethanol. Linearity of the emission intensity with the concentration, limiting detectable sample concentrations, and Stokes shifts are reported.

Glafenine↗