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J Chromatogr A

Title:		Comparison of analytical and semi-preparative columns for high-performance liquid chromatography-solid-phase extraction-nuclear magnetic resonance
Author(s):		Miliauskas G; van Beek TA; de Waard P; Venskutonis RP; Sudholter EJ;
Address:		"Laboratory of Organic Chemistry, Natural Products Chemistry Group, Wageningen University, Dreijenplein 8, 6703 HB Wageningen, The Netherlands. giedrius.miliauskas@wur.nl"
Journal Title:		J Chromatogr A
Year:		2006
Volume:		20051220
Issue:		1-Feb
Page Number:		276 - 284
DOI:		10.1016/j.chroma.2005.11.059
ISSN/ISBN:		0021-9673 (Print) 0021-9673 (Linking)
Abstract:		"The application of analytical and semi-preparative columns in reversed-phase liquid chromatography-solid-phase extraction-nuclear magnetic resonance (HPLC-SPE-NMR) was compared. The work was aiming at separating a higher sample amount in a single run and in this way to reduce the necessary NMR measurement time of separated compounds. Several parameters for compound separation and trapping procedures were optimised: flow rate of HPLC and make-up water pumps, choice of stationary phase cartridges and drying time. The separation and loadability of nine model compounds on analytical and semi-preparative columns was determined, as well as the focussing capacity of SH-type SPE cartridges. It was found that a semi-preparative column--or multiple peak trapping on analytical columns--gave better results than a standard 4.6mm analytical column for non-polar compounds (e.g. flavonoid aglycones, sesquiterpene lactones, non-polar terpenes, logP>2), but for polar compounds (logP<-2) did not offer any advantage over an analytical column, or was even disadvantageous. For intermediately polar compounds (-2
Keywords:		"Amygdalin/analysis Caffeine/analysis Chemical Fractionation/*instrumentation/methods Chromatography, High Pressure Liquid/*instrumentation/*methods Gallic Acid/analysis Glucosinolates/analysis Nuclear Magnetic Resonance, Biomolecular/methods Oils, Volatil;"
Notes:		"MedlineMiliauskas, Giedrius van Beek, Teris A de Waard, Pieter Venskutonis, Rimantas P Sudholter, Ernst J R eng Comparative Study Research Support, Non-U.S. Gov't Netherlands 2005/12/21 J Chromatogr A. 2006 Apr 21; 1112(1-2):276-84. doi: 10.1016/j.chroma.2005.11.059. Epub 2005 Dec 20"