Synthesis and characterization of novel internal surface reversed-phase silica supports for high-performance liquid chromatography |
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Authors: | Gasparrini Francesco Ciogli Alessia D'Acquarica Ilaria Misiti Domenico Badaloni Elena Giorgi Fabrizio Vigevani Aristide |
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Institution: | Dipartimento di Studi di Chimica e Tecnologia delle Sostanze Biologicamente Attive, Università La Sapienza, P.le Aldo Moro 5, 00185 Rome, Italy. francesco.gasparrini@uniroma1.it |
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Abstract: | An original synthetic method was developed for the preparation of a family of six novel deactivated restricted-access materials (RAMs), belonging to the group of the internal surface reversed-phase (ISRP) supports. The supports (ISRP-RAM phases A-F) have an alkyl-chain (14 methylenes) with two embedded ureido groups bound only to the internal surfaces of the porous silica, and polyvinyl alcoholic groups (PVA, 100,000-->22,000 molecular weight) chemically bound to the external surfaces. The average pore diameters of the prepared ISRP-RAM supports, calculated by inverse size-exclusion chromatography, ranged between 49 A and 88 A, and were able to exclude macromolecules heavier than about 24000 Da (such as serum proteins) from the pores. The novel supports were designed for the determination of a semi-synthetic anticancer drug of the camptothecin family in human plasma, but they represent universal ISRP-RAM supports not limited to such class of compounds. |
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