Characterisation of reversed-phase stationary phases for the liquid chromatographic analysis of basic pharmaceuticals by thermodynamic data.

This paper describes the characterisation of reversed-phase liquid chromatography (RPLC) columns using thermodynamic measurements. Retention versus 1/T data were used to construct Van't Hoff plots. The slope of these plots indicates the standard enthalpy of transfer of the analyte from the mobile to the stationary phase. The standard entropy can be calculated from the intercept. Van't Hoff plots were linear for the investigated RPLC columns, meaning that for basic analytes over the temperature range studied no changes in the retention mechanism occurred. Enthalpies and entropies of transfer of basic analytes from the mobile to the stationary phase revealed information about the types of interaction of protonated and neutral compounds with the stationary phases. However, a clear view using the present set of basic compounds on how these thermodynamic data may explain the observed substantial differences in peak symmetry cannot be given. It is considered that addition of N,N-dimethyloctylamine (DMOA) to the eluent will results in a dynamically coating of the stationary phase. Addition of DMOA to the eluent resulted for protonated basic compounds in a reduction of both enthalpy and entropy. In practice, with DMOA in the eluent symmetrical peaks were obtained. It is assumed that this is due to blocking residual silanols and/or ion exclusion effects.

Characterisation of reversed-phase liquid chromatography stationary phases for the analysis of basic pharmaceuticals: eluent properties and comparison of empirical test methods.

The reversed-phase liquid chromatographic analysis of basic pharmaceuticals can be problematic. Both the properties of the eluent and the stationary phase can influence the chromatographic performance. Therefore selection of suitable experimental conditions for the analysis of basic compounds can be difficult. This paper shows that the organic modifier and the nature of the buffer influence the eluent properties. Moreover, the nature and amount of modifier also influence the basicity of the analytes. Investigations showed that the nature of the buffer can have a significant influence on retention and peak shape of basic compounds. Test procedures using basic analytes as test probes provided relevant information with respect to selecting columns to analyse basic pharmaceutical compounds. Test procedures using compounds like aniline, phenol and benzene were found to be less suitable.

A new pneumatic pump for extracorporeal circulation: TPP (true pulsatile pump). Experimental and first clinical results.

A pulsatile, membrane type pump, TPP, was developed for use in routine cardiac surgery. The artificial ventricle consists of a polycarbonate housing with an inlet and outlet polyurethane tricuspid valve. The membrane is actuated hydraulically. For pre-clinical studies, we designed a study in sheep. After a pump run of 6 hours the animals were allowed to recover and sacrificed after 72 hours. All clinical parameters returned to normal values (p > 0.05 vs. control values). During pump run we found elevated free plasma hemoglobine. However, these values returned to normal until the end of the observation period. Thereafter, the device was used in ten routine cardiac surgery procedures. All patients survived the procedure and were discharged from hospital. The postoperative course of lab parameters (kidney, liver and blood count) was no different to routine cardiac surgical procedures. This pulsatile pump system can thus be safely employed in cardiac surgery.

Mechanical unloading properties of axial flow pumps and their effect on myocardial stunning.

Postischemic myocardial dysfunction affects morbidity and mortality in patients with coronary artery disease. It is known that mechanical unloading of the left heart ventricle can positively influence postischemic myocardial dysfunction. In this respect we tested two miniaturised axial flow pumps, i.e. the 14-F and the 21-F Hemopump. An experimental study was carried out on 30 open chest sheep where regional myocardial wall motion was followed using sonomicrometry in a preparation of transient coronary artery occlusion. Only the larger 21-F Hemopump showed hemodynamically significant unloading of the left ventricle. Furthermore, as far as stunning is concerned, systolic wall thickening recovered better when this type of pump was used during reperfusion. Also postejection thickening, which is an indication of diastolic postischemic dysfunction, is reduced significantly in the postischemic area (ANOVA, p < 0.05). Thus, the 21F Hemopump, but not the 14F Hemopump, provides adequate mechanical unloading in order to beneficially influence myocardial stunning.

Gel permeation for the on line removal of proteins from plasma samples prior to HPLC.

Gel permeation chromatography (GPC) has been investigated for the on line removal of proteins from plasma samples prior to their analysis by HPLC. The results show that GPC is a mild and effective way to remove proteins from plasma samples. It can very well be coupled on line to HPLC, providing the solutes are suitable for preconcentration on the analytical column itself or on a small pre-column, after the GPC. Under these conditions excellent reproducibility and accuracy can be obtained.

Minicomputers in homeopathy

Repertory analysis of homoeopathic cases has always been very time-consuming. For this reason homoeopathic doctors have often had to restrict themselves to searching for the most likely remedies from a total of... (AU)