The GBE product was obtained after the eluant
was concentrated and dried, then weighted.
The neutral lipid fraction was redissolved in n-hexane after removal of the C-I eluant
and transferred to fresh Bond Elut columns to elute cholesteryl esters with n-hexane and finally to elute TAGs with n-hexane containing 1% diethylether and 10% dichloromethane (by vol).
Bis(glycinato)copper(II) [[Cu[([L.sub.2]).sub.2]].sub.2] (3.11 g, 0.01 M) column eluted with water gave blue eluant
. Yield: 1.92 g, 63%; d.p.: 212[degrees]C; UV-Vis (nm): 296, 386, 628.
The diluted extracting solution was chromatographed with HZ816 macroreticular resin using a gradient eluant
of [H.sub.2]O-ethanol ([H.sub.2]O, 10%, 30%, 60%, and 90% ethanol).
The reaction mixture was refluxed for 2.5 h, and then the solvent was evaporated and the residue purified by column chromatography using Si[O.sub.2] as adsorbent and petroleum ether purified as eluant
and its purity was > 98% using the HPLC methods described in a later section.
The resin which had adsorbed Pb(II) was shaken with the eluant
. After reaching equilibrium, the concentration of Pb(II) in the aqueous phase was determined and then the percentage of elution was obtained.
After drying with [Na.sub.2]S[O.sub.4] and concentrating under reduced pressure, the EtOAc phase (2 g) was chromatographed over Sephadex LH-20 (30 x 2 cm), using MeOH as the eluant
. This procedure provided 42 fractions (15 mL each), which were pooled into four groups (I-IV), after TLC analysis.
The oil obtained after extraction was purified by flash chromatography using silica gel (60 g) as the stationary phase and hexane: diethyl ether (80:20) as the eluant
to yield 7.8 g of colorless, catalyst-free conjugated soybean oil.
was an unbuffered mixture of ethanol and water at a flow rate of 0.5 ml/min (except in the case of Potassium Fluoride when it was set at 1.0 ml/min).
Therefore, 0.01 M NaOH was used as eluant
for desorption studies.
The sample injected and eluant
of acetonitrile: water 9:1 was pumped at the rate of 1 mL/min in column controlled at 55[degrees]C.
The solvent was removed under reduced pressure and the residue was purified by flash chromatography, using dichloromethane/hexane 6/4 as eluant
, to give 4 as a dark yellow solid (66.1 mg; yield 65%).