Fluid extraction

M. A. McHugh and V. J. Knikonis, Supercritical Fluid Extraction, Butterworth Pubhshers, Stoneham, Mass., 1986. 

Cascara sagrada is used as a cathartic. It is most useful when prepared as a fluid extract, and tends to be a mild laxative causing Htfle discomfort. However, on prolonged use it may result in characteristic melanotic pigmentation of the rectal mucosa. The bitter taste can be lessened, owing to neutralization of the acid constituents, if the ground substance is moistened and mixed with magnesium or calcium hydroxide. This treatment may lessen the potency of the preparation. 

Supercritical Fluid Extraction. Supercritical fluid (SCF) extraction is a process in which elevated pressure and temperature conditions are used to make a substance exceed a critical point. Once above this critical point, the gas (CO2 is commonly used) exhibits unique solvating properties. The advantages of SCF extraction in foods are that there is no solvent residue in the extracted products, the process can be performed at low temperature, oxygen is excluded, and there is minimal protein degradation (49). One area in which SCF extraction of Hpids from meats maybe appHed is in the production of low fat dried meat ingredients for further processed items. Its apphcation in fresh meat is less successful because the fresh meat contains relatively high levels of moisture (50). 

The concern by consumers about cholesterol has stimulated the development of methods for its removal. Three principal approaches are in the pilot-plant stages use of enzymes, supercritical fluid extraction, and steam distillation. Using known techniques, it is not possible to remove all cholesterol from milk. Therefore, FDA guidelines identify cholesterol-free foods as containing less than 2 mg cholesterol per serving, and low cholesterol foods as containing from 2 to 20 mg (37). 

Dosage forms of naturally occurring materials having therapeutic activity are prepared by extractive processes, especially percolation and maceration. Examples of such dosage forms have included certain tinctures, symps, fluid extracts, and powdered extracts. 

Purifications of elfamycins have been described in the Hterature using Craig distribution (2,34), chromatography on Sephadex LH-20 (2,14,26) and Amberlite XAD-2 (10,17,19,26), supercritical fluid extraction (37), and chromatography on an Ito multilayer cod planet centrifuge (26,38). and nmr assignments of most elfamycins have been accompHshed (3,24,26,32). The characteristic uv spectra permits some differentiation (12) and bathochromic shifts associated with Al " complexation have been used to quantify efrotomycin (2, R = CH ) in feed premixes (39,40). 

Removing an analyte from a matrix using supercritical fluid extraction (SEE) requires knowledge about the solubiUty of the solute, the rate of transfer of the solute from the soHd to the solvent phase, and interaction of the solvent phase with the matrix (36). These factors collectively control the effectiveness of the SEE process, if not of the extraction process in general. The range of samples for which SEE has been appHed continues to broaden. Apphcations have been in the environment, food, and polymers (37). 

The development of methods of analysis of tria2ines and thek hydroxy metabohtes in humic soil samples with combined chromatographic and ms techniques has been described (78). A two-way approach was used for separating interfering humic substances and for performing stmctural elucidation of the herbicide traces. Humic samples were extracted by supercritical fluid extraction and analy2ed by both hplc/particle beam ms and a new ms/ms method. The new ms /ms unit was of the tandem sector field-time-of-flight/ms type. 

Separation Techniques. Current methods for separating fatty acids are by solvent crystaUi2ation or by the hydrophili2ation process. Other methods that have been used in the past, or perhaps could be used in the future, are panning and pressing, solvent extraction, supercritical fluid extraction, the use of metal salts in assisting in separation, separations using urea complexes, and adsorption/desorption. 

FIG. 22-19 Schematic diagram of a typical supercritical fluid-extraction process. 

Adsorption and Desorption Adsorbents may be used to recover solutes from supercritical fluid extracts for example, activated carbon and polymeric sorbents may be used to recover caffeine from CO9. This approach may be used to improve the selectivity of a supercritical fluid extraction process. SCF extraction may be used to regenerate adsorbents such as activated carbon and to remove contaminants from soil. In many cases the chemisorption is sufficiently strong that regeneration with CO9 is limited, even if the pure solute is quite soluble in CO9. In some cases a cosolvent can be added to the SCF to displace the sorbate from the sorbent. Another approach is to use water at elevated or even supercritical temperatures to facilitate desorption. Many of the principles for desorption are also relevant to extraction of substances from other substrates such as natural products and polymers. 

Analytical Supercritical Fluid Extraction and Chromatography Supercritical fluids, especially CO9, are used widely to extrac t a wide variety of solid and hquid matrices to obtain samples for analysis. Benefits compared with conventional Soxhlet extraction include minimization of solvent waste, faster extraction, tunabihty of solvent strength, and simple solvent removal with minimal solvent contamination in the sample. Compared with high-performance liquid chromatography, the number of theoretical stages is higher in... 

The influence of soil ageing on the recovery of POPs from spiked soil samples was also assessed. Spiked lettuce samples were subjected to in vitro gastrointestinal extraction to assess the bioavailability of Endosulfan compounds. All samples (soil and lettuce) were extracted using pressurised fluid extraction and analysed using gas chromatography with mass selective detection. 

COMPARISON OF ESSENTIAL OIL COMPOSITION OF SALVIA MIRZAYANII OBTAINED BY SUPERCRITICAL FLUID EXTRACTION AND HYDRODISTILLATION METHODS... 

Supercritical fluid extraction (SFE) has been widely used to the extraction processes in pharmaceutical industries. Besides application of SFE in phannaceuticals, it has been applied on a wide spectmm of natural products and food industries such as natural pesticides, antioxidants, vegetable oil, flavors, perfumes and etc [1-2]. 

The thermo- and chemolabilc genuine valepotriates arc not present in the usual therapeutically used formulations (infusion, extract, fluid extract, tincture),... 

Supercritical fluid extraction (SFE) and Solid Phase Extraction (SPE) are excellent alternatives to traditional extraction methods, with both being used independently for clean-up and/or analyte concentration prior to chromatographic analysis. While SFE has been demonstrated to be an excellent method for extracting organic compounds from solid matrices such as soil and food (36, 37), SPE has been mainly used for diluted liquid samples such as water, biological fluids and samples obtained after-liquid-liquid extraction on solid matrices (38, 39). The coupling of these two techniques (SPE-SFE) turns out to be an interesting method for the quantitative transfer... 

Unfortunately, not much experimental work has been carried out on the combination of Supercritical fluid extraction and liquid chromatography systems (43, 44). One of the reasons for this arises from the difficulties in achieving compatibility between the extraction solvent and the FC mobile phase. Baseline perturbations have been... 

ON-LINE COUPLING OF SUPERCRITICAL FLUID EXTRACTION WITH CAPILLARY ELECTRODRIVEN SEPARATION TECHNIQUES (SFE-CESTs)... 

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