PubMed · 6837318
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M Kata, M Wayer, E György. 1983. [Microcapsulation by spray drying].. https://pubmed.ncbi.nlm.nih.gov/6837318/
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Microcapsules were prepared from human serum albumin (HSA) by interfacial cross-linking with terephthaloyl chloride (TC). TC concentrations were increased from 0.5 to 5% w/v, while pH (9.8) and reaction time (30 min) were kept constant. Fourier transform infrared (FT-IR) spectra of lyophilized microcapsules were compared. Correlations were established with microcapsule morphology and size. The results were compared with those of previous studies exploring pH or reaction time and with those of parallel determinations of microcapsule free amino groups. With 0.5% TC, decreases of the ester-assigned 1724-cm-1 band area and of the carboxylate-assigned 1394-cm-1 band area were observed compared with pure HSA. This phenomenon was attributed to a removal of contaminating lipids of HSA. Increasing TC concentration resulted in a progressive increase of the band areas at 1724 cm-1 (esters) and 1795 cm-1 (anhydrides), in a further decrease of the 1394-cm-1 band area (carboxylates), and in marked alterations of teh 1340-1080-cm-1 region. These changes, which revealed the progressive acylation of hydroxy and carboxylate groups of HSA, were accompanied by an increase of the 1624-cm-1 band area (beta-sheet), reflecting interchain H-bonding due to cross-linking. As observed in the previous studies of pH and reaction time, important spectral changes corresponded to low values of -NH2 content, to a decrease in microcapsule mean size (from > 30 to < 15 microns), and to modifications of the membrane surface (made rough).
The separation of phenylbutazone (PB) and its major metabolite oxyphenbutazone (OPB) using supercritical fluid chromatography (SFC) has been investigated. The separations were studied on octadecylsilane, silica and cyano packed columns with 5% methanol in carbon dioxide as mobile phase and detection at 240 nm. The octadecylsilane column showed the most favourable chromatographic parameters for the analysis of the analytes. Recoveries of PB and OPB from spiked human serum were in the 82-83% range using solid phase extraction on an ODS cartridge. Limits of detection of the SFC assay were 0.1 microgram ml-1 for PB and 1.0 microgram ml-1 for OPB. Accuracy and precision of the method were in the 0.24-4.94% range for PB and OPB. The SFC method was directly comparable to an HPLC assay of the same analytes. The SFC method was also applied to a commercial 100 mg dosage form of PB with good recovery of PB.
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