Liquid solid extraction combined with

SFE was also more selective as compared to the liquid solid extraction (LSE) with isopropanol, chloroform, and isopropanol-chloroform. Glycolipids and phospholipids were found in the LS extract but they were not extracted by SFE. The SF extracts were also cleaner than the LS extracts and did not require the various clean up procedures required by the latter extraction method. The SF extracts were richer in fatty acids whereas, the isopropanol-chloroform combined extracts were richer in the more polar and hi molecular weight lipids. 

There is a great number of separation and purification processes to choose from in process development, but classical separations such as crystallization, filtration, drying, liquid-liquid extraction and distillation are still predominantly used. For solid products crystallization, filtration, and drying are the first options although vacuum distillation and extraction combined with the other techniques are also possible. For liquid products, liquid-liquid... 

Reprocessing is based on liquid-liquid extraction for the recovery of uranium and plutonium from used nuclear fuel (PUREX process). The spent fuel is first dissolved in nitric acid. After the dissolution step and the removal of fine insoluble solids, an organic solvent composed of 30% TriButyl Phosphate (TBP) in TetraPropylene Hydrogenated (TPH) or Isopar L is used to recover both uranium and plutonium the great majority of fission products remain in the aqueous nitric acid phase. Once separated from the fission products, back-extraction combined with a reduction of Pu(I V) to Pu(III) allows plutonium to be separated from uranium these two compounds can be recycled.2... 

Fattahi, N., S. Samadi, Y. Assadi, and M. R. M. Hosseini. 2007. Solid-phase extraction combined with dispersive liquid-liquid microextraction-ultra preconcentration of chlorophenols in aqueous samples. J. Chromatogr. A 1169 63-69. 

Classical liquid-liquid and liquid-solid extractions are recently receiving additional examination, as new injection techniques for GC have made very simple, low-volume extractions feasible. Recently, several commercial systems for large-volume liquid injections (up to 150 pL all at once, or up to 1 to 2 mL over a short period of time) have become available. When combined with robotic sampling systems, these have become powerful tools in the trace analysis of a variety of sample types. Due to its simplicity, classical liquid-liquid extraction is often the method of choice for sample preparation. Some of the robotic samplers available for this type of analysis, such as the LEAP Technologies Combi-PAL robotic sampler, which has been licensed by several instrument vendors, are also capable of performing automated SPME and SHE. 

Fernandez MDR, Wille SMR, Samyn N, Wood M, Lopez-Rivadulla M, De Boeck G (2009) On-line solid-phase extraction combined with liquid chromatography-tandem mass spectrometry for high throughput analysis of 1 l-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid in urine. J Chromatogr B 877(22) 2153—2157. doi 10.1016/j.jchromb.2009.04.047... 

The total elapsed time is substantially less with SFE extraction than with conventional liquid-solid extractions. Moreover, the hands-on time required of the operator for the pre-extraction steps prior to SFE (5-10 minutes) would be only a fraction of the total hands-on sample preparation time required by employing tradition preparation processes (30 minutes) - an advantage over traditional methods. In the case of the vitamin-A active compounds, the extraction and analysis for four samples with two replicates each (a total of 8 extractions and 8 analyses) using the conventional manual method requires 4 hours. For the combined SFE and analyses for the 8 extractions and 8 analyses, the total elapsed time is 3 hours. However, until an operator has worked with both SFE and traditional liquid-solid sample preparation, it is not obvious that the operator intervention (or hands-on) time is much different. It is estimated that this may be as much as 70 % of the 4 hours in the traditional method and as little as 10 % in the 3 hours of the SFE method. 

METHOD FOR THE DETERMINATION OF SOME SELECTED STEROID HORMONES AND BISPHENOL A IN WATER AT LOW NG/L LEVEL BY ON-LINE SOLID-PHASE EXTRACTION COMBINED WITH LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY... 

Sioufi, A. Richard, J. Mangoni, R Godbillon, J. Determination of diclofenac in plasma using a fully automated analytical system combining liquid-solid extraction with liquid chromatography. J.Chromatogr., 1991, 565, 401-407 [plasma SPE pharmacokinetics LOQ 31 nM]... 

An alternative to liquid-solid extraction is supercritical fluid extraction (SEE) which allows the extraction of analytes from solid samples, i.e., marine sediments, to be performed faster and more efficiently since these have a lower viscosity and higher diffusivity than liquid solvents." CO2 is the most widely used supercritical fluid with or without a modifier, e.g., methanol and toluene. SFE can be combined with solid-phase trapping.Compared with Soxhlet extraction, SFE gave similar yields, but the extracts were much cleaner and it was not necessary to clean the extracts before GC analysis."" ... 

Jen HC, Lin SJ, Tsai YH, Chen CH, Lin ZC, Hwang DF. Tetrodotoxin poisoning evidenced by solid-phase extraction combining with liquid chromatography-tandem mass spectrometry. J Chromatogr B 2008 871 95-100. 

During the last few years, miniaturization has become a dominant trend in the analysis of low-level contaminants in food and environmental samples. This has resulted in a significant reduction in the volume of hazardous and expensive solvents. Typical examples of miniaturization in sample preparation techniques are micro liquid/liquid extractions (in-vial) and solvent-free techniques such as solid-phase microextraction (SPME). Combined with state-of-the-art analytical instrumentation, this trend has resulted in faster analyses, higher sample throughputs and lower solvent consumption, whilst maintaining or even increasing assay sensitivity. 

White phosphorus (15.5 g, 0.5 g-atom) was cut into approximately 0.1-g pieces under water, washed with acetone followed by ether, and then added in one portion to the reaction mixture. The reaction mixture consisted of 1.0 mol of phenyl lithium in 750 ml of diethyl ether. The exothermic reaction was continued by heating at reflux for 3 h. Water was then added to hydrolyze the remaining organometallic this resulted in the precipitation of a yellow solid. The solid was removed by filtration, and the two phases of the remaining liquid portion were separated. The aqueous portion was extracted with three 50-ml portions of diethyl ether, which were combined with the organic layer, dried over anhydrous sodium sulfate, and evaporated to give the product phenylphosphine in 40% yield. 

Dai S. et al., 2005. Quantitation of sifuvirtide in monkey plasma by an online solid-phase extraction procedure combined with liquid chromatography/electrospray ionization tandem mass spectrometry. Rapid Commun Mass Spectrom 19 1273. 

Hogenboom A.C., Niessen W.M.A., and Brinkman U.A., 1999a. Online solid-phase extraction-short-column liquid chromatography combined with various tandem mass spectrometric scanning strategies for the rapid study of transformation of pesticides in surface water. J Chromatogr A 841 33. 

In addition, a novel fluorous support has been developed recently as an alternative to traditional polymer supports and applied successfully to oligosaccharide synthesis in combination with the trichloroacetimidate method [541]. Each intermediate in the fluorous oligosaccharide synthesis [542,543] could be obtained by simple fluorous-organic solvent extraction, and the reactions could be monitored by TLC, NMR and MS, in contrast to solid-phase reactions. Moreover, the new liquid-phase technique is anticipated to be easily applicable to the large-scale synthesis. 

Fish. Solid biota samples, mainly fish, should be quickly killed by liquid N2 [28] or cervical dislocation [32] and kept at low temperatures (— 20°C). Some authors preferred desiccation of the sample at high temperature (70°C) [33,34] or lyophylisation [28]. The extraction and isolation steps would be combined when using lyophylisation and homogenisation, followed by a Soxhlet extraction, usually with MeOH, and a subsequent solid-phase extraction (SPE) clean-up, prior to the quantification. 

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