CRYSTALLIZATION OF LIPIDS
(typical conditions given)
From
|
T Celsius
|
Monacylglycerides
|
|
dichloromethane/ethanol/water (40:20:1)
|
18
|
slow cooling from 40 C to 18 C
|
|
dichloromethane/ethanol/water (3:2:0.15)
|
20
|
Clear supernatant was kept in a sealed tube at 20 C over a period of several weeks.
|
|
water-free diethylether-ethanol (10:1)
|
|
Crystals are highly hygroscopic and were handled in a dry nitrogen atmosphere.
|
|
flash chrom. (5% boric acid/silica gel, hexane /ethyl acetate = 95:5)
|
42.5
|
single crystals obtained in ethyl acetate by slow evaporation at 4 C
|
|
petroleum spirit
|
20-40
|
crystals are biaxial positive & frequently twined on the planes.
|
|
dichloromethane/ethane/water
|
< 8
|
crystal are in needles.
|
|
dichloromethane/ethane/water
|
20
|
crystals are thin plates
|
|
|
|
Diacylglycerides
|
|
ether/ethanol/water
|
14
|
Crystals redissolved above 22 C. Flocculent precipitate. Monoclonic crystals with two molecules in the asymmetric unit
|
|
diethyl ether/ethanol/water (10:1:0.05)
|
12
|
Minor impurities removed by diethyl ether/ethanol soln. Needle-like single crystals
|
|
a solution in hexane
|
|
Crystal obtained by slow evaporation of the solvent
|
|
dichloromethane/methane (2:1)
|
|
Induced by vapor diffusion of diethylether. Thin lanceolate crystals
|
|
ethyl acetate
|
4
|
Flash chromatography and slow evaporation
|
|
|
|
Triacylglycerides
|
|
petroleum spirit
|
40-60
|
purified by chromatography on aluminium oxide column
|
|
petroleum ether
|
39.4-53.2
|
in thick plates. Crystals are triclinic
|
|