Ultrasonic-aided extraction

He et al. (2002) used an off-line HPLC/CE method to map cancer cell extracts. Frozen ovarian cancer cells (containing 107 cells) were reconstituted in 300 pL of deionized water and placed in an ultrasonic bath to lyse the cells. Then the suspension was centrifuged and the solubilized proteins were collected for HPLC fractionation. The HPLC separation was carried out on an instrument equipped with a RP C-4 column, 250 mm x 4.6 mm, packed with 5-pm spherical silica particles. Extracted proteins were dissolved in 300 pL of DI water, and lOOpL was injected onto the column at a flow rate of 1 mL/min. Buffer A was 0.1% TEA in water and buffer B was 0.1% TFA in acetonitrile. A two-step gradient, 15-30% B in 15 min followed by 30-70% B in 105 min, was used. The column effluent was sampled every minute into a 96-well microtiter plate with the aid of an automatic fraction collector. After collection, the fractions were dried at room temperature under vacuum. The sample in each well was reconstituted before the CE analysis with 10 pL deionized water. The... 

Sonication helps improve solid-liquid extractions. Usually a finely ground sample is covered with solvent and placed in an ultrasonic bath. The ultrasonic action facilitates dissolution, and the heating aids the extraction. There are many EPA methods for solids such as soils and sludges that use sonication for extraction. The type of solvent used is determined by the nature of the analytes. This technique is still in widespread use because of its simplicity and good extraction efficiency. For example, in research to determine the amount of pesticide in air after application to rice paddy systems, air samples collected on PUF were extracted by sonication, using acetone as the solvent. The extraction recoveries were between 92% and 103% [21]. 

In the conventional method, the shard powder (or visible residue, or soil) is extracted with three separate aliquots of c. 0.5 ml DCM MeOH (dichlor-omethane methanol 1 1, v/v), with ultrasonication for 5 minutes to break up any particle aggregates and to aid dissolution. The solvent is separated from any insoluble material (including the ceramic) with centrifugation (5 minutes at lOOOrpm) and each of the three solvent aliquots is combined into a new clean vial. The solvent is then removed by placing the sample under a stream of nitrogen on a warm hotplate to aid evaporation, leaving the extracted... 

In sediment and soil samples, the isomers of cresol are determined by transferring a small portion of the solid sample (1 g) to a vial and adding methylene chloride. The contaminants are extracted from the sample with the aid of an ultrasonic probe. The methylene chloride extract is filtered, concentrated, and subjected to GC/MS analysis for quantitation. 

Another example of ultrasound use is leaching of organic impurities from different kinds of samples. The main analytes of interest are PAHs, which are widespread in soil, sediment, dust, and particulate samples [55]. USE is recommended as a fast, efficient, and direct environmental sample preparation method for determination of PCBs, nitrophenols, pesticides, or polymer additives. Organometallic and biologically active compounds (such as vitamins A, D, and E) present in samples in trace quantities, can be extracted from animal and plant tissues with the aid of ultrasonic wave energy [59]. Table 6.6 presents some typical applications of USE in trace analysis of biological and environmental samples [60]. 

Pesticides such as atrazine and simazine have also been extracted from honey with the aid of an ultrasonic bath. In addition to the type of extractant, variables such as the extractant volume, sonication time and number of extraction cycles were optimized, the temperature and the height of the transmitting liquid in the bath being kept constant. A comparison of the ensuing method with its shake-flask extraction counterpart showed the former to be faster and more efficient, and provide relatively lower standard deviations [9]. 

Recently, polymeric ultrafiltration membranes were used for degumming crude soybean oil and removing phospholipids from the crude oil/hexane miscella (168). Crude soybean oil also can be de-acidified by methanol extraction of the free fatty acids and the extract separated into fatty acids and solvent by a membrane filter (169). A surfactant-aided membrane degumming also has been applied to crude soybean oil, and the degummed oil contained 20-58 ppm of phosphorus (170). Supercritical carbon dioxide extraction was shown to be an effective means of degumming (171). In this process, soybean oil countercurrently contacted supercritical carbon dioxide at 55 MPa and 75°C. The phosphorus content of the oil was reduced from 620 ppm to less than 5 ppm. Ultrasonic degumming was also successfully used to reduce the gum content of soybean oil (172). 

The use of ultrasounds to aid the extraction is another possibility. Phthalates (Abb et al. 2009) and perfluorinated alkanoic acid (PEA) (Kato et al. 2009) determinations have been reported. Ethyl acetate (phthalates) or formic acid with methanol (perfluoroalkyl chemicals) was added to the dust sample, and extraction was performed in an ultrasonic bath at room temperature for 10 min. In the case of phthalates an enrichment step was not carried out to avoid the risk of contamination. Pyrethroids and their metabolites can also been extracted from indoor dust samples by adding methylene chloride followed by sonication for 10 min (Starr et al. 2008). Another option is the combination of Soxhlet extraction with an ultrasonic treatment (Schecter et al. 2009). 

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