Original PaperPilot-scale ion-exchange centrifugal partition chromatography: Purification of sinalbin from white mustard seedsThe purification of p-hydroxybenzylglucosinolate (sinalbin) on a multigram scale from a crude aqueous extract of white mustard seeds (Sinapis alba var. concerta) was successfully achieved by scaling up a strong ion-exchange centrifugal partition chromatography (SIXCPC) laboratory procedure. Thus, the one-step sinalbin purification was performed with 2.35 g of crude extract in l170 min (830 mg/h) up to 70.3 g in l160 min (26.3 g/h) by switching from a 200 mL laboratory scale column to a 5.7 L pilot-scale column. The required biphasic solvent system contained ethyl acetate, nbutanol, and water in 3:2:5 v/v/v proportions, Aliquat 336m (trioctylmethyl ammonium chloride) was added to the organic stationary phase (80 mM) and acted as ionexchanger. Potassium iodide in the aqueous mobile phase (80 mM) was used as sinalbin displacer. The 28.5 mass scale factor arose from the increase in mobile phase flow-rate (from 2 to 50 mL/min), from the higher mass of injected white mustard seed extract (from 12 to 350 g), and from the calculated productivity (from 830 mg to 26.3 g). These results demonstrate that industry scale production of glucosinolates is easily performed by SIXCPC, thus providing pure reference standards for pharmacology studies.
A quercitrin rich vegetal flavonoid sample was fractionated using a new hydrodynamic CCC apparatus based on the It0 scheme IV design. The Kromaton CCC apparatus has two spools with a tube coiling allowing work with two different apparatus volumes. The small "analytical" volume was 94 mL and the large "preparative" volume was 1.07 L. The fractionation of the flavonoid sample was done using the two machine volumes. The bi phasic liquid system was a non chlorinated solvent system, butanonelwater. W detection was possible at 330 nm. In one run, 330 mg of the flavonoid sample could be fractionated by the CCC machine in six peaks that were collected in nine fractions. 3003 Copyright 0 1998 by Marcel Dekker, Inc. www.dekker.com Downloaded by [Erciyes University] at 22:57 02 January 2015 3004 BERTHOD ET AL.The HPLC and MS analysis of the fractions allowed identification of the main constituents of the sample. Quercitrin, a rhamno-flavonoid, was the major compound making up more than 88% wlw of the studied sample. The three minor identified flavonoids were quercetin, kaempferol, and kaempferol-3-rhamnoglucoside. Six very minor impurities were detected by the HPLC analysis of the fractions, but they were not unambiguously identified.
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