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Pilot‐scale ion‐exchange centrifugal partition chromatography: Purification of sinalbin from white mustard seeds
Author(s) -
Toribio Alix,
Nuzillard JeanMarc,
Pinel Benoît,
Boudesocque Leslie,
Lafosse Michel,
De La Poype François,
Renault JeanHugues
Publication year - 2009
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200800651
Subject(s) - chromatography , ion chromatography , chemistry , ion exchange , partition (number theory) , ion , mathematics , organic chemistry , combinatorics
Abstract The 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 ˜170 min (830 mg/h) up to 70.3 g in ˜160 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, n ‐butanol, and water in 3:2:5 v/v/v proportions, Aliquat 336® (trioctylmethyl ammonium chloride) was added to the organic stationary phase (80 mM) and acted as ion‐exchanger. 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.