Supercritical assisted phase method

When using supercritical fluids in place of liquids (non-solvent),an advanced, and greener, manufacturing approach to induce precipitation of the polymer can be achieved. This approach is commonly named the supercritical assisted phase inversion method (SAPIM) (Cardea et al, 2010). 

In liquid-solid extraction (LSE) the analyte is extracted from the solid by a liquid, which is separated by filtration. Numerous extraction processes, representing various types and levels of energy, have been described steam distillation, simultaneous steam distillation-solvent extraction (SDE), passive hot solvent extraction, forced-flow leaching, (automated) Soxh-let extraction, shake-flask method, mechanically agitated reflux extraction, ultrasound-assisted extraction, y -ray-assisted extraction, microwave-assisted extraction (MAE), microwave-enhanced extraction (Soxwave ), microwave-assisted process (MAP ), gas-phase MAE, enhanced fluidity extraction, hot (subcritical) water extraction, supercritical fluid extraction (SFE), supercritical assisted liquid extraction, pressurised hot water extraction, enhanced solvent extraction (ESE ), solu-tion/precipitation, etc. The most successful systems are described in Sections 3.3.3-3.4.6. Other, less frequently... 

Supercritical fluid extraction (SFE), microwave-assisted extraction (MAE) and Soxhlet extraction under various experimental conditions were applied for spiked poly(vinyl) chloride samples. Extracted dyes were separated in an ODS column (250 X 4.6 mm i.d. particle size 5 jum) using methanol as the mobile phase. Dyes are well separated by this method as demonstrated in Fig. 3.59. The optimal parameters of the extraction methods are compiled in Table 3.23. Recoveries depended on both the type of extraction method and the chemical structure of the dye. It was found that the highest recovery can be obtained by MAE and the extraction efficacy was the lowest for Solvent red 24 [129],... 

The impact of the extraction conditions using various solvents on the recoveries has never been studied in detail, and the results have never been compared. The introduction of modern extraction methods, such as microwave-assisted extraction, supercritical fluid extraction, and solid-phase extraction, probably will improve the efficiency of extraction, even in the instance of unstable pigments and pigment mixtures. The majority of TLC separations were carried out on traditional silica layers. As the chemical structures and, consequently, the retention characteristics of pigments are highly different, a wide variety of eluent systems has been employed for their separation, consisting of light petroleum, ethyl formate, ethyl acetate, benzene, toluene, chloroform, methanol, n-butanol, formic or acetic acid, and so forth. 

In this introductory book chapter, several modem extraction techniques will be described, including supercritical fluid extraction, pressurized liquid extraction, pressurized hot Avater extraction, microwave assisted extraction, membrane-assisted solvent extraction, solid phase micro extraction and stir-bar sorptive extraction. These are techniques that meet many of today s requirements in terms of environmental sustainability, speed and automation. Basic principles of operation as well as method optimization will be discussed and compared for the different techniques. Both analytical and industrial applications will be discussed, together with commercial instruments available on the market. Key references will be given, and conclusions regarding applicability of the different techniques with respect to sample e, target-molecules and analytical vs. large-scale applications. 

There are many sample preparation procedures published in the scientific literature, and within the scope of this chapter, only the most current and popular methods will be discussed. By far, the commonest and most popular method used for pretreatment of liquid samples is solid phase extraction (SPE) [40,41]. For solid samples, several techniques are available including supercritical fluid extraction (SFE) [42,43], microwave-assisted solvent extraction (MASE) [44,45] and accelerated solvent extraction (ASE) [46,47]. Solvent extraction methods have long been established as the standard approach to sample preparation, but the increasingly demanding needs of industries like the pharmaceutical, agrochemical and petrochemical for greater productivity, faster assays, and increased automation have led to the development of newer ways of sample preparation summarised in Fig. 2.3. 

Solid-phase extraction (SPE) using small, disposable cartridges, columns, or disks is employed for isolation and cleanup of pesticides from water and other samples prior to TLC analysis, especially using reversed-phase (RP) octa-decyl (C-18) bonded silica gel phases. Microwave-assisted extraction (MAE) is a time- and solvent-saving method for removing residues from samples such as soils. Supercritical fluid extraction (SEE) has been used for sample preparation in the screening of pesticide-contaminated soil by conventional TLC and automated multiple development (AMD). Ultrasonic solvent extraction (USE) and videodensitometry have been combined for quantification of pesticides in sod. Matrix solid-phase dispersion (MSPD) with TLC and GC has been used to determine diazinon and ethion in nuts. 

For many years, the traditional sample preparation methods, such as the Soxhlet extraction, were applied. Most of these methods have been used for more than 100 years, and they mostly require large amounts of organic solvents. These methods were tested during those times, and the analysts were familiar with the processes and protocols required. However, the trends in recent years are automation, short extraction times, and reduced organic solvent consumption. Modern approaches in solid sample preparation include microwave-assisted solvent extraction (MASE), pressurized liquid extraction, accelerated solvent extraction (ASE), matrix solid-phase dispersion (MSPD), automated Soxhlet extraction, supercritical fluid extraction (SEE), gas-phase extraction, etc. 

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). 

Although most official methods for pesticide analysis in water samples use liquid-liquid extraction (LLE) on account of its simplicity and consolidated status, solid-phase extraction (SEE) techniques have gained increasing popularity lately. Other methodologies including solid-phase microextraction (SEME), liquid-phase microextraction (LFME), supercritical fluid extraction (SEE), and microwave-assisted extraction (MAE) have been used to determine pesticides in water [5,28,30]. 

Saponins from plant materials can be extracted using different techniques and solvents. The conventional techniques for saponin extraction used soxhlet, liquid-liquid or solid-liquid extraction (Berhow et al. 2002 Hassan et al. 2010a, b). These methods consume a lot of solvent, time and may lead to potentially deleterious degradation of labile compounds (Kerem et al. 2005). Therefore, in recent years, new extraction techniques include accelerated solvent extraction, supercritical fluid extraction, solid-phase microextraction, sonication, extraction with supercritical or subcritical water, and microwave-assisted extraction have been developed and are considered to be more efficient than the conventional methods (Wu et al. 2001 Kerem et al. 2005 Ligor et al. 2005 Gii lii-Ustundag and Mazza 2007). Ultrasonication-assisted extraction of ginseng saponins was about three times faster than the liquid-liquid extraction and can be carried out at lower temperature (Wu et al. 2001). Kerem et al. (2005) reported that methanol- microwave assisted method to extract saponin of chiclqtea proved to be faster and more efficient than soxhlet extraction. 

---