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Biomedical subjects

Pieter Dehouck

Publications and source records attributed to Pieter Dehouck.

6 recordsLinked to original sources

Precision study on capillary electrophoresis methods for metacycline.

A CE method for metacycline (MTC) determination was investigated in an inter-laboratory experiment. Many problems were encountered in this study, most of which were related to the transfer of the method to different CE equipment. The reported problems could be classified into different categories: problems related to the precision, to the parameters in the protocol, and to the MTC peak shape. As the peak shape problem was partially responsible for the poor precision, a new CE method was developed in order to obtain a good MTC peak shape on all equipment. The precision of this new method for MTC determination was examined in an intermediate precision study, where the influence of the factors "time" and "equipment" was investigated. Although the new method could be transferred to different instruments, the precision remained poor mainly due to the contributions of the between-replicate and the between-injection variances.

Anti-Bacterial Agents↗

Investigation of degradation products in a topical gel containing erythromycin and benzoyl peroxide by liquid chromatography-mass spectrometry.

Benzamycin, combining benzoyl peroxide and erythromycin, is a topical gel used in the treatment of acne vulgaris. Because of the reactivity of benzoyl peroxide, preparations containing both erythromycin and benzoyl peroxide might be unstable and degradation products could be formed. To investigate and identify these latter products, a gradient-based liquid chromatographic method using volatile mobile phase constituents was developed. Mass spectrometry data were acquired on solutions containing erythromycin and benzoyl peroxide and on freshly prepared, 2-month-old and 18-month-old samples of Benzamycin. With the reference spectra as interpretative templates, it was concluded that erythromycin undergoes oxidation, followed by benzoylation.

Benzoyl Peroxide↗

Facilitated column selection in pharmaceutical analyses using a simple column classification system.

In this paper, the performance of a previously developed classification system applied to pharmaceutical chromatographic analyses, is investigated. The separation of seven different drug substances from their respective impurities was studied. The chromatographic procedure for acetylsalicylic acid, clindamycin hydrochloride, buflomedil hydrochloride, chloramphenicol sodium succinate, nimesulide and phenoxymethylpenicillin was performed according to the corresponding European Pharmacopoeia (Ph. Eur.) monograph. The separation of dihydrostreptomycin sulphate was performed according to the literature. It is shown that the column ranking system is a helpful tool in the selection of a suitable column in these analyses.

Aspirin↗

Characterisation of reversed-phase liquid-chromatographic columns by chromatographic tests comparing column classification based on chromatographic parameters and column performance for the separation of acetylsalicylic acid and related compounds.

Selection of RP-LC columns with suitable selectivity for a given analysis is difficult. For example, the European Pharmacopoeia (Ph. Eur.) and other official compendia for drug analysis only give a general description of the stationary phase in the operating procedure of a liquid chromatographic method. The need for a general test method to characterise RP-LC columns has been rising since the 1970s. A project to define a chromatographic procedure characterising RP-LC columns was started earlier. A procedure to measure test parameters was introduced and a classification of the columns, based on a minimal number of parameters, was obtained. This paper focuses on correlating the column classification with the selectivity obtained for a real separation. The separation of acetylsalicylic acid (aspirin) and related compounds was performed according to the Ph. Eur. monograph on the stationary phases previously characterised chromatographically. It was examined whether the classes of columns, determined using test parameter results, contain either suitable or unsuitable supports for the aspirin separation. The system suitability test prescribed by the Ph. Eur. in order to distinguish between suitable or unsuitable columns for this separation was also evaluated.

Aspirin↗

Intermediate precision study on a capillary electrophoretic method for chlortetracycline.

We describe an intermediate precision study on a capillary electrophoretic (CE) method for chlortetracycline. It is shown how in one setup the influence of the factors time, analyst, and equipment on the precision can be investigated. As different types of CE equipments were included, the transferability of the method could be examined. Both the qualitative and quantitative aspect of the method were investigated. It was shown that small adaptations in method conditions can have a large influence on the method transferability. Although the method could be transferred to different types of CE equipments, the precision of the method was found poor when the between-equipment variability was taken into account. Despite the use of an internal standard, the between injection variability was found rather high.

Chlortetracycline↗

Characterisation of reversed-phase liquid chromatographic columns by chromatographic tests. Rational column classification by a minimal number of column test parameters.

The European Pharmacopoeia (Ph. Eur.) and other official compendia give only a general description of the stationary phase in the description of a liquid chromatographic method. Therefore the selection of a column giving suitable selectivity presents difficulties. Earlier, a test procedure was proposed that allows to measure 36 chromatographic parameters which have been described for characterising stationary phases. This procedure was carried out on 69 reversed-phase liquid chromatography (RP-LC) columns. This paper focuses on the classification of RP-LC stationary phases based on chromatographic parameters. A chemometric study was conducted using 24 parameters that could be measured in a repeatable and reproducible way. Principal component analysis was used to classify the columns and to estimate the minimal number of parameters necessary for a rational classification. It is shown that after reducing the number of parameters from 24 to four or three, similar classifications were obtained. The column classifications were compared to the European Pharmacopoeia stationary phase description and to the column properties obtained from the manufacturers.

Chromatography, Liquid↗