Focused microwave-assisted solvent extraction

Two main types of MAE systems are commercially available, in both cases agitation is provided during extraction to improve the mass transfer phenomenon. In closed extraction vessels, extraction is performed under controlled pressure and temperature. In focused microwave-assisted solvent extraction (FMASE), only a part of the extraction vessel containing the sample is irradiated with microwaves. Instrumental setups like Soxwave combine both the features of Soxhlet and the advantages of microwave, thus making extraction an even more attractive alternative to traditional solid—liquid extraction. 

Work is in progress to validate the MAE method, proposed for EPA, in a multi-laboratory evaluation study. Nothing similar has been reported for additives in polymeric matrices. Dean el al. [452] have reviewed microwave-assisted solvent extraction in environmental organic analysis. Chee et al. [468] have reported MAE of phthalate esters (DMP, DEP, DAP, DBP, BBP, DEHP) from marine sediments. The focus to date has centred on extractions from solid samples. However, recent experience suggests that MAE may also be important for extractions from liquids. 

The improvements in Soxhlet extractions are high-pressure Soxhlet extraction (HPS), automated Soxhlet extraction (Soxhlet HT and Buchi B811) and focused microwave-assisted Soxhlet extraction (Soxwave and FMASE) as shown by Luque de Castro MD and Garcia-Ayuso in 1998. The solvents used for extraction are polar species (dimethyl formamide,... 

New developments in Soxhlet extraction have been applied to the analysis of PAHs in soils and sediments. " Focused Microwave-Assisted Soxhlet Extraction (FMASE) uses focused microwave irradiation to achieve agitation in the sample. The application of microwaves drastically reduces extraction time ( 1 h) and solvent use. Recoveries of PAHs were reported to be 11 to 101 % in the extraction step and no filtering was necessary prior to analysis. 

In Figure 7.53 a flow-injection interface for fluorometric monitoring of focused microwave-assisted Soxhlet extraction is represented [195]. This assembly allows real-time online monitoring of the PAHs extracted from solid samples in each Soxhlet cycle and provides qualitative and semi-quantitative information from natural and spiked samples. The method has been applied to a certified reference material (CRM 524, BCR, industrial soil/organics) for quality assurance/validation. The proposed technique is as efficient as conventional Soxhlet to extract PAHs from soils but with a drastic reduction of both extraction time and organic solvent disposal. 

General trends are focused on reduced-solvent extractions or adsorption-based methods — enviromnentaUy friendly solvents for both solid and liquid samples. In recent decades, advanced techniques like supercritical fluid extraction (SFE), ° pressurized liquid extraction (PLE)," microwave-assisted extraction (MAE), ultrasound-assisted extraction, countercurrent continued extraction (www.niroinc.com), solid... 

Fig. 5.8. (A) General scheme of a dynamic focused microwave-assisted extractor. (B) Experimental set-up used to integrate microwave-assisted extraction with the subsequent steps of the analytical process. (1) Leaching step CT controller, MO microwave oven, S sample, R condenser, WR water reservoir, TCPP two-channel piston pump, ER extract reservoir, SV switching valve. (2) Clean-up/preconcentration step M methanol, A air, B buffer, PP peristaltic pump, F filter, EL elution loop, MC mini-column, R retention direction, E elution direction, 1V1-1V3 injection valves, W waste. (3) Individual separation-detection step HPIV high-pressure injection valve, AC analytical column, DAD diode array detector, SR solvent reservoirs.

A, acaricide AV, avicide I, insecticide F, fungicide H, herbicide GR, growth regulator N, nematocide R, rodenticide US, ultrasonication LLE, liquid-liquid extraction CU, cleanup ImCU, immuno cleanup SPE, solid-phase extraction MSPD, matrix solid-phase dispersion SBSE, stir bar sorptive extraction SD, steam distillation FMSE, focused microwave Soxhiet extraction PFE, pressurized fluid extraction ASE, assisted solvent extraction ScFE, subcritical fluid extraction SFE, supercritical fluid extraction SEC, size-exclusion chromatography LC, liquid chromatography (fraction collection) LTLP, low temperature lipid precipitation. 

Li, H., Chen, B., Nie, L., and Yao, S. 2004. Solvent effects on focused microwave assisted extraction of polyphenolic acids from Eucommia ulmodies. Phytochemical Analysis, I5(5) 306-312. 

Weichbrodt et reported on the use of focused open-vessel microwave-assisted extraction (EOV-MAE) for the determination of organochlorine pesticides in high-moisture samples such as fish. The results were comparable to those with closed-vessel microwave-assisted extraction (CV-MAE) and ASE. The main advantage of FOV-MAE is that the use of Hydromatrix is unnecessary as the solvent mixture of ethyl acetate and cyclohexane allows the removal of water from the sample matrix via azeotropic distillation. 

Methods involve extractions of analytes into organic solvents, as well as treatments with acidic or basic reagents. Solid-phase extraction can be used for removal and pre-concentrations of analytes in aqueous solutions. Applications of low-power focused microwave technology have been investigated as a means of dissolution, and good results have been reported for extractions of organometal-lic compounds of tin and mercury (Schmitt et al., 1996 Szpunar et al., 1996). Analyses of CRMs were used for verification. The time necessary for quantitative isolations of the analytes was greatly reduced, e.g. 24 h to 5 min. In addition, there were reductions in solvent volumes, and improvement in analyte recoveries. Some of the analytical procedures for speciation of particular elements such as mercury, described later in this chapter, include microwave-assisted sample preparation. 

Microwave-assisted extractions (MAE) can be performed in open (focused MAE) or closed (pressurized MAE) flasks. This technique is commonly used for extractions from complex and difficult sample matrices, replacing time- and solvent-intensive Soxhlet extractions or hydrodistillations.46 MAE is also widely applied to environmental samples, for example, for extracting polycyclic aromatic hydrocarbons (PAH) from soil, methylmercury from sediments, and trace metals and pesticide residues from plant material47 48 The use of microwave treatment instead of hydrodistillation offers a solvent-free separation technique essential oils are heated and dry-distilled 46... 

This chapter covers techniques for the extraction of semivolatile organics from solid matrices. The focus is on commonly used and commercially available techniques, which include Soxhlet extraction, automated Soxhlet extraction, ultrasonic extraction, supercritical fluid extraction (SFE), accelerated solvent extraction (ASE), and microwave-assisted extraction (MAE). The underlying principles, instrumentation, operational procedures, and selected applications of these techniques are described. In a given application, probably all the methods mentioned above will work, so it often boils down to identifying the most suitable one. Consequently, an effort is made to compare these methodologies. 

The focus in Chapters 7 and 8 is on the specific sample preparation approaches available for the extraction of organic compounds from environmental matrices, principally soil and water. Chapter 7 is concerned with the role of Soxhlet, ultrasonic and shake-flask extraction on the removal of organic compounds from solid (soil) matrices. These techniques are contrasted with newer developments in sample preparation for organic compound extraction, namely supercritical fluid extraction, microwave-assisted extraction and pressurized fluid extraction. Chapter 8 is arranged in a similar manner. Initially, details are provided on the use of solvent extraction for organic compounds removal from aqueous samples. This is followed by descriptions of the newer approaches, namely solid-phase extraction and solid-phase microextraction. 

Accelerated solvent extraction (ASE), focused microwave soxhiet extraction (FMSE), immuno affinity cleanup (im-Cu), liquid-liquid extraction (LLE), low-temperature lipid precipitation (LTLP), matrix solid-phase dispersion (MSPD), microwave-assisted extraction (MAE), nanofiltration (NF), pressurized fluid extraction (PEE), single drop microextraction (SOME), solid-phase extraction (SPE), solid-phase microextraction (SPME), steam distillation (SD), stir bar sorptive extraction (SBSE), surpercritical fluid extraction (SFE), subcritical fluid extraction (ScFE), supported liquid membrane extraction (SLME), ultra-sonication (US), size exclusion chromatography (SEC), liquid chromatography-fraction collection (LC)... 

In this context, studies about the development of relevant analytical methods allowing the detection of pesticide residues in VOO are usually focused on an optimization of the various steps of the analysis process, namely extraction, clean-up, identification, and quantitation of pesticide content. The common extraction methods are Soxhlet extraction, microwave-assisted extraction (MAE), supercritical fluid extraction (SEE), and accelerated solvent extraction (ASE). Cleanup methods include SPE, matrix solid-phase dispersion (MSPD), and gel permeation chromatography (GPC). 

The solvent technique for concentrating surfactants is not discussed here. See Ref. [40] for details. Morales-Munoz et al. discuss a screening method for LAS in sediments. It is based on water Soxhlet extraction assisted by focused microwaves. The extractor is coupled with an online preconcentrator/derivatization/detection manifold through a flow injection interface [107]. 

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