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United States Department of Agriculture

Agricultural Research Service

Research Project: DISCOVERY AND DEVELOPMENT OF NATURAL PRODUCTS FOR PHARMACEUTICAL AND AGROCHEMICAL APPLICATIONS

Location: Natural Products Utilization Research

Title: Preparation and application of reversed phase chromatorotor for the isolation of natural products by centrifugal preparative chromatography)

Author
item Ilias, Muhammad
item Samoylenko, Vladimir
item Machumi, Francis
item Zaki, Mohamed
item Gillum, Van
item Hetta, Mona

Submitted to: Journal of Chromatography A
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 2/1/2013
Publication Date: 3/15/2013
Citation: Ilias, M., Samoylenko, V., Machumi, F., Zaki, M.A., Gillum, V. 2013. Preparation and application of reversed phase chromatorotor for the isolation of natural products by centrifugal preparative chromatography. Journal of Chromatography A. 8(3):311-314.

Interpretive Summary: The art of centrifugal chromatography is hindered by unavailability of appropriate method and rotors for reversed phase (RP) separation. This research had a purpose of developing a method for reversed phase centrifugal chromatography and demonstrating its application in separation of organic molecules. RP rotor plates (Chromatorotors) were successful prepared; using binder free RP solid SiO2 sorbent layers of different thicknesses, packed between two supported circular glass discs. The Chromatorotors were made compatible with the existing devices for centrifugal chromatography; and were used successfuly to separate two polar diastereoisomeric alkaloids (1 and 2) and saponin glycosides (3 and 4) in a preparative scale.

Technical Abstract: A method of preparation of Chromatorotor or plates with a reversed phase (RP) solid silica gel sorbent layer has been developed for preparative centrifugal chromatography. The RP-rotor plates consist of binder free RP solid SiO2 sorbent layers of different thicknesses paked between two supported circular glass discs and can be used in any appropriate device for Centrifugal Chromatography. Polar organic compounds with close Rf values as well as extracts and column fractions were separated and /or purified in a preparative scale using the prepared RP-rotors, eluted with different solvent systems, including mixtures of aqueous-based solvents. Using-custom made RP-Chromatorotors, two polar diastereoisomeric alkaloids (1 and 2) and saponin glycosides (3 and 4) were separated in a preparative scale. The method was seen to be economical both in terms of instrumentation and accessories; as well as fast, efficient and environmentally friendly.

Last Modified: 8/24/2016
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