Feeds extraction procedures

Since lupin seeds are used in some areas in cattle feeding, it is of practical as well as theoretical interest to determine the stage at which the seeds will be rich in the alkaloidal material responsible for toxicity. It has also been important to devise methods for the removal of alkaloids from the seeds so that the detoxified or debittered material can still be used as feed (111). Extraction procedures which accent the recovery of non-alkaloidal material have less interest to the alkaloid chemist than those which provide for the isolation of the pure organic bases. Given below are typical examples of the extraction procedures employed for the isolation of the lupin alkaloids lupinine, cytisine, Z-sparteine, d-lupanine, and anagyrine. The methods selected are representative of those utilized for the isolation of the less abundant or well-known lupin alkaloids as well. These methods are also representative of the different quantities of materials which are handled. One of the methods was selected (for anagyrine) to indicate some of the complexities of separation when there are a number of alkaloids present in a plant, rather than only one main alkaloidal constituent. The techniques of fractional distillation of the bases, fractional crystallization of alkaloid salts, such as perchlorates and picrates, and extractions dependent upon differential solubility have been employed for the isolation of pure individual alkaloids from a mixture. 

The quality characteristics of the oil produced by the enzyme-assisted aqueous extraction process is comparable to that of conventional extraction procedures except in its phosphorus content (Table 12.5). The enzymatic process yields oil with less phosphorus which requires no or limited degumming. The crude oil from this process can be physically refined without further treatment (Laiho et al., 1991). Despite this improved quality of the crude oil which is an apparent cost saving in subsequent downstream processing, the enzymatic process has not been commercially exploited due to problems with yields. Considerable degree of emulsification occurs during the process. Approximately 18-25% of the available oil in the seed remains unrecovered in a standard operation. The discovery that the versatile protein, oleosin, binds approximately 20% of the oil in oil-bearing seeds (Tzen et al., 1990) has implicated this protein in the low yields associated with this process. Thus, the recoveries could be improved by the use of proteases. It has, however, been observed that successful application of proteases to improve oil recovery produces excessively bitter meals, repressing the potential utilization of the meal as feed or food. 

It is characteristic of unsteady-state operation that concentrations at any point in the apparatus change with time. This may result from changes in concentrations of feed materials, flow rates, or conditions of temperature or pressure. In any case, batch operations are always of the unsteady-state type. In purely batch operations, all the phases are stationary from a point of view outside the apparatus, i.e., no flow in or out, even though there may be relative motion within. The familiar laboratory extraction procedure of shaking a solution with an immiscible solvent is an example. In semibatch operations, one phase is stationary while the other flows continuously in and out of the apparatus. As an example, we may cite the case of a drier where a quantity of wet solid is contacted continuously with fresh air, which carries away the vaporized moisture until the solid is dry. 

An equihbrium, or theoretical, stage in liquid-liquid extraction as defined earlier is routinely utilized in laboratory procedures. A feed solution is contacted with an immiscible solvent to remove one or more of the solutes from the feed. This can be carried out in a separating funnel, or, preferably, in an agitated vessel that can produce droplets of about 1 mm in diameter. After agitation has stopped and the phases separate, the two clear liquid layers are isolated by decantation. 

After a single-stage liquid-liquid contact the phase remaining from the feed sohition (raffinate) can be contacted with another quantity of fresh extraction solvent. This crosscurrent extraction scVieme (Fig. 15-4) is an excellent laboratoiy procedure because the extrac t and raffinate phases can be analyzed after each stage to generate equihbrium data. Also, the feasibility of solute removal to lowTevels can be demonstrated. 

Because estrogenic mycotoxins usually occur at microgram per kilogram (pg/kg) levels there is special interest in analytical procedures for reliable detection of zearalenone and its metabolites between 10 and 100 pg/kg. In response to the risk of a great economic loss to the industry and the threat to human health as a result of exposure to zearalenone, several methods have been developed for the quantification of zearalenone and its metabolites in different foods, feeds, animal tissues, blood and urine. Detailed reviews have been given by Steyn et al. 1991 Betina 1993 Frisvad and Thrane 1993 Scott 1993 Steyn 1995 and Lawrence and Scott 2000. The determination of zearalenone in cereals can be divided into five steps grinding of the sample, extraction of the sample, clean-up, separation and detection. 

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