A two-step method was developed for the preparation of food-grade wax. The first step involved the solventdefatting of crude wax, which gave a dark brown, dry, powdered wax with a m.p. of 75-79°C. The major impurity in the defatted wax was the dark brown resinous matter. In the second step, the resinous matter was removed by bleaching with sodium borohydride in isopropanol. This step yielded a pale yellow, odorless wax with purity higher than 99% and with a m.p. of 80-83°C. The resinous matter was a mixture of aliphatic aldehydes, fatty alcohols, and FA. High-temperature GC analysis of the purified rice bran wax indicated that it contained 11 major and 9 minor types of saturated wax esters. The major and minor peaks contained C 44 -C 64 and C 45 -C 59 wax esters, respectively. Rice bran wax was mainly a mixture of saturated esters of C 22 and C 24 FA and C 24 to C 40 aliphatic alcohols, with C 24 and C 30 being the predominant FA and fatty alcohol, respectively. The alcohol portion of the wax esters also contained small amounts of branched and odd carbon number fatty alcohols.
An efficient synthesis of 3,4-dihydropyrimidines using bismuth chloride as a catalyst from an aldehyde, b-keto ester and urea in acetonitrile is described. Compared to the classical Biginelli reaction conditions, this new method consistently has the advantage of good yields (56-97%).
A simple method for the isolation of γ-oryzanol from rice bran acid oil has been developed. The
basis of the present isolation protocol is calcium ion induced precipitation of anionic micellar
aggregates. Rice bran acid oil, a byproduct of rice bran oil processing industries, is subjected to
conventional vacuum distillation to remove free fatty acids. Aqueous alkaline hydrolysis of the
resultant residue, upon dilution with water, produces anionic micellar aggregates containing
solubilized γ-oryzanol. Addition of calcium ions to this aqueous micellar aggregate induces instant
coprecipitation of the calcium salts of the fatty acids and the aggregate-associated γ-oryzanol. The
dried precipitate is extracted with ethyl acetate. Ethyl acetate is evaporated from the extract, and
γ-oryzanol is purified from the residue by silica gel column chromatography. Experimental details
for the isolation and characterization procedure are described. The present method will give ready
access to the physiologically beneficial and value-added pharmaceutical product γ-oryzanol.
Keywords: γ-Oryzanol; ferulic acid esters; CAD esters; HPLC; LSIMS
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