Extraction techniques with aqueous solvents

Certain aqueous materials can be extracted directly with a solvent to prodice an aroma concentrate. This technique has found utility in studies on wine aroma (3 ). The investigators studied model wine systems containing 12% ethanol and 4.4% sucrose. Extractions were performed manually, and the organic solutions were concentrated under vacuum. They concluded that Freon 11 (bp 24°) was the solvent of choice if the organic essence is to be stored for an extended period of time, they recommended methylene chloride as the solvent. The presence of sugar did not create any difficulties. 

In 1965, the Dubna workers found a longer-lived lawrencium isotope, 256Lr, with a half-life of 35 s. In 1968, Thiorso and associates at Berkeley used a few atoms of this isotope to study the oxidation behavior of lawrencium. Using solvent extraction techniques and working very rapidly, they extracted lawrencium ions from a buffered aqueous solution into an organic solvent — completing each extraction in about 30 s. 

Membrane separation coupled on-line to a flow-injection system was employed for the monitoring of propazine and terbutryn in natural water. A microporous hydro-phobic membrane was utilized in which the analytes were extracted from the aqueous medium into an organic solvent that was carried to the flow cell of a photodiode-array spectrophotometer. The LCDs were 4-5 qg so the technique could potentially be used for screening purposes. Samples with positive detection would require further analysis. 

Solutes have differing solubilities in different liqnids dne to variations in the strength of the interaction of solnte molecnles with those of the solvent. Thus, in a system of two immiscible or only partially miscible solvents, different solutes become unevenly distribnted between the two solvent phases, and as noted earlier, this is the basis for the solvent extraction technique. In this context, solvent almost invariably means organic solvent. This uneven distribution is illustrated in Fig. 1.3, which shows the extractability into a kerosene solution of the different metals that appear when stainless steel is dissolved in aqueous acid chloride solution. The metals Mo, Zn, and Fe(III) are easily extracted into the organic solvent mixture at low chloride ion concentration, and Cu, Co, Fe(ll), and Mn at intermediate concentration, while even at the highest chloride concentration in the system, Ni and Cr are poorly extracted. This is used industrially for separating the metals in super-alloy scrap in order to recover the most valuable ones. 

The technique of CPC was also employed as a key step in the purification of 26 phenolic compounds from the needles of Norway spruce (Picea abies, Pinaceae). An aqueous extract of needles (5.45 g) was separated with the solvent system CHCl3-Me0H-i-Pr0H-H20 (5 6 1 4), initially with the lower phase as mobile phase and then subsequently switching to the upper phase as mobile phase. Final purification of the constituent flavonol glycosides, stilbenes, and catechins was by gel filtration and semipreparative HPLC. °... 

In principle, an extraction technique involving pH adjustment of the aqueous phase can offer purification similar to ion exchange chromatography. Although the method uses a smaller volume of solvent, it has limited ability to remove low-level impurities. Therefore, the replacement of ion exchange chromatography with extraction requires some ingenuity. 

The handling and disposal problems associated with the use of liquid solvent extractors have resulted in increased attention to the separation and preconcentration of organic compounds in water by collection in synthetic polymers followed by elution with an organic solvent (2). For example, selective collection and concentration of organic bases on methylacrylic ester resin from dilute water samples have been reported (3). Such collection techniques are especially well-suited to flow-injection measurement techniques. In this study, ionizable organic analytes such as salicylic acid and 8-hydroxyquinoline (oxine) were extracted into a polymer and then back extracted by an aqueous solution. Amperometric measurement using a flow-injection technique was employed to monitor the process. 

Silica columns can tolerate relatively heavy loads of triglyceride and other nonpolar material. Such material is not strongly adsorbed and can easily be washed from the column with 25% diethyl ether in hexane after a series of analyses (83). Procedures for determining vitamins A and E have been devised in which the total lipid fraction of the food sample is extracted with a non-aqueous solvent, and any polar material that might be present is removed. An aliquot of the nonpolar lipid extract containing these vitamins is then injected into the liquid chromatograph without further purification. Direct injection of the lipid extract is possible because the lipoidal material is dissolved in a nonpolar solvent that is compatible with the predominantly nonpolar mobile phase. Procedures based on this technique are rapid and simple, because there is no need to saponify the sample. 

For phenolics in fruit by-products such as apple seed, peel, cortex, and pomace, an HPLC method was also utilized. Apple waste is considered a potential source of specialty chemicals (58,62), and its quantitative polyphenol profile may be useful in apple cultivars for classification and identification. Chlorogenic acid and coumaroylquinic acids and phloridzin are known to be major phenolics in apple juice (53). However, in contrast to apple polyphenolics, HPLC with a 70% aqueous acetone extract of apple seeds showed that phloridzin alone accounts for ca. 75% of the total apple seed polyphenolics (62). Besides phloridzin, 13 other phenolics were identified by gradient HPLC/PDA on LiChrospher 100 RP-18 from apple seed (62). The HPLC technique was also able to provide polyphenol profiles in the peel and cortex of the apple to be used to characterize apple cultivars by multivariate statistical techniques (63). Phenolic compounds in the epidermis zone, parenchyma zone, core zone, and seeds of French cider apple varieties are also determined by HPLC (56). Three successive solvent extractions (hexane, methanol, aqueous acetone), binary HPLC gradient using (a) aqueous acetic acid, 2.5%, v/v, and (b) acetonitrile fol-... 

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