Existing HPLC methods determine only pure gossypol whereas the official AOCS method determines both gossypol and other physiologically active gossypol‐like compounds that react with 3‐amino‐1‐propanol and aniline. The feed industry uses the official AOCS method, which is complex and produces results that do not correlate well among laboratories. HPLC methods were developed, using 3‐amino‐1‐propanol as a complexing agent, for the quantitative determination of free and total gossypol in cottonseed meal, oil, and ethanolic miscella. These methods are simple, sensitive, and provide reproducible results. In addition the use of toxic aniline is eliminated.
Extraction of rice bran lipids with supercritical carbon dioxide (SC-CO 2 ) was performed. To investigate the pressure effect on extraction yield, two isobaric conditions, 7000 and 9000 psi, were selected. A Soxhlet extraction with hexane (modified AOCS method Aa 4-38; 4 h at 69°C) was also conducted and used as the comparison basis. Rice bran with a moisture content of 6%, 90% passable through a sieve with 0.297 mm opening, was used for extraction. A maximum rice bran oil (RBO) yield of 20.5%, which represents 99+% lipid recovery, was obtained with hexane. RBO yield with SC-CO 2 ranged between 19.2 and 20.4%. RBO yield increased with temperature at isobaric conditions. At the 80°C isotherm, an increase in RBO yield was obtained with an increase in pressure. The pressure effect may be attributed to the increase in SC-CO 2 density, which is closely related to the value of the Hildebrand solubility parameter. RBO extracted with SC-CO 2 had a far superior color quality when compared with hexane-extracted RBO. The level of sterols in SC-CO 2 -extracted RBO increased with pressure and temperature. JAOCS 75, 623-628 (1998).
Commercial processing of cottonseed requires hexane to extract and recover edible oil. Gossypol and aflatoxin are not removed from extracted meals. A bench‐top extraction process with 95% (vol/vol) aqueous ethanol (EtOH) solvent has been developed that extracts all three of the above materials with a much less volatile solvent. In this process, cottonseed is pretreated and extracted with ambient 95% EtOH to remove gossypol and then extracted with hot 95% EtOH to extract oil and aflatoxin. Membranes and adsorption columns are used to purify the various extract streams, so that they can be recycled directly. A representative extracted meal contained a total gossypol content of 0.47% (a 70% reduction) and 3 ppb aflatoxin (a 95% reduction). Residual oil content was approximately 2%. Although the process is technically feasible, it is presently not economical unless a mill has a continual, serious aflatoxin contamination problem. However, if a plant cannot meet the hexane emission standards under the Clean Air Act of 1990, this process could provide a safer solvent that may expand the use and increase the value of cottonseed meal as a feed for nonruminants.
The critical moisture content of cottonseed flakes extracted with an aqueous alcohol solvent can be defined as that flake moisture level at which the flakes lose no moisture during extraction. This study shows that the critical moisture content for aqueous ethanol (92%, w/w) is 3%. For aqueous isopropanol (88%, w/w) this value is 6%. If the moisture contents of the flakes are above these levels, then the solvents pick up moisture. For moisture contents below this level, the flakes adsorb moisture and actually dry the alcohol. It is proposed that this latter capability can be used as a basis for a method to control water accumulation in aqueous alcohol solvent extractions.
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