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High resolution glass capillary columns with chemically bonded stationary phases: application to the gas chromatographic analysis of sterols and steroids in biological extracts

1981; Wiley; Volume: 58; Issue: 1 Linguagem: Inglês

10.1007/bf02666057

1558-9331

C. Madani, E.M. Chambaz,

Mass Spectrometry Techniques and Applications

Abstract A new approach has been developed for the preparation of highly stable glass capillary columns using irreversible bonding of polysiloxane polymers to the glass surface. The general procedure involves (a) synthesis of reactive linear polysiloxanes from variously (alkyl, aryl) substituted dichlorosilanes through homologous or heterologous polymerization under alcaline aqueous conditions, and (b) covalent condensation of the polymers to a properly prepared glass capillary surface at high temperature. The principle has been first applied to the successful preparation of apolar gas chromatographic systems (methylpolysiloxanes), then extended to the obtention of polar systems (methyl phenyl polysiloxanes). The flexibility of the approach is demonstrated by the possibility of obtaining stationary phases of various and controlled polarity (i.e., extent of phenyl substitution), tailor‐made to a given analytical problem. These gas Chromatographic systems appear to be remarkably stable both with time and temperature up to 300 C and compare favorably to existing systems for their high resolution properties. These columns have been satisfactorily used in the last years for the analysis of sterols and steroids of biological origin and most extensively in the study of urinary steroid metabolite in humans under pathological conditions.