ABSTRACT
An approach to speed up the isolation of hydrophilic metabolites in complex natural matrixes by using a HLB/MCX-HPLC/MS system based on the retention properties of hydrophilic-lipophilic and cation exchange polymeric cartridges was developed. This methodology was successfully applied to the re-isolation of small water soluble compounds with completely different structures from two different natural extracts such as a dipeptide (vanchrobactin) from a bacterium culture broth and a pyrrolidine bearing a carboxylic acid moiety (clionapyrrolidine A) from a sponge. This method improved not only the efficiency of the isolation methodology but also the isolation time in relation to the existing methods.
Subject(s)
Chromatography, High Pressure Liquid/methods , Chromatography, Ion Exchange/methods , Complex Mixtures/chemistry , Mass Spectrometry/methods , Siderophores/isolation & purification , Animals , Cations/chemistry , Hydrophobic and Hydrophilic Interactions , Peptides/isolation & purification , Porifera , Pyrrolidines/isolation & purification , Vibrio , WaterABSTRACT
Careful selection of both high-pH mobile phase as well as organic modifier, was performed in order to develop and optimize HPLC conditions for the separation of drug discovery compounds. High-pH mobile phases provide excellent chromatographic resolution and increased mass loading of basic compounds. The analytical methods so defined have been successfully transferred to preparative automated UV-directed purification, an important fact due to the increasing number of samples requiring purification. It should be noted that, the single prerequisite for this approach is an analytical LC-UV-MS run, therefore the system has the ability to collect only fractions likely to contain the target product. A cost-effective strategy for maximizing the purification of drug discovery compounds is proposed.
Subject(s)
Chromatography, High Pressure Liquid/methods , Hydrogen-Ion ConcentrationABSTRACT
A new secosterol (1), along with pachyclavulariaenone B (3), was isolated from Pachyclavularia violacea. The structures of these compounds were established on the basis of the NMR and MS experiments.
Subject(s)
Cnidaria/chemistry , Secosteroids/isolation & purification , Animals , Chromatography, High Pressure Liquid , Colonic Neoplasms , Drug Screening Assays, Antitumor , Humans , Indonesia , Leukemia P388 , Lung Neoplasms , Mass Spectrometry , Melanoma , Mice , Molecular Conformation , Molecular Structure , Nuclear Magnetic Resonance, Biomolecular , Secosteroids/chemistry , Secosteroids/pharmacology , Stereoisomerism , Tumor Cells, Cultured/drug effectsABSTRACT
Two new xeniolides, xeniolide-F (1) and 9-hydroxyxeniolide-F (2), along with isoxeniolide-A (3) and 7,8-oxido-isoxeniolide-A (4), have been isolated from Xenia sp. and their structures established on the basis of extensive NMR and MS studies.
