Gel adsorption chromatography

The enantioselective determination of 2,2, 3,3, 4,6 -hexachlorobiphenyl in milk was performed by Glausch et al. (21). These authors used an achiral column for an initial separation, followed by separation of the eluent fraction on a chiral column. Fat was separated from the milk by centrifugation, mixed with sodium sulfate, washed with petroleum ether and filtered. The solvent was evaporated and the sample was purified by gel permeation chromatography (GPC) and silica gel adsorption chromatography. Achiral GC was performed on DB-5 and OV-1701 columns, while the chiral GC was performed on immobilized Chirasil-Dex. 

Separation, Characterization and Analysis of the Distillate Fractions. Results from the analyses of the <200° C coal-liquid distillates (after removal of trace quantities of acids and bases) are summarized in Table IV. Results from the dual silica-gel/alu-mina-gel adsorption chromatography separations of the 200° to 325° C, 325° to 425° C, and 425° to 540° C coal-liquid distillates are summarized in Table V. Data for the acid and base extracts of the polyaromatic-polar adsorption fractions are also included in Table V. Summary data on analysis of the saturate fractions are listed in Table VI. Data in Table VI show a trend toward higher percentages of zero- and one-ring saturates in lower-rank coals. 

Function of Pre-HPLC Column. The schematic in Figure 6 for a HPLC chromatogram representative of extracts of agricultural products illustrates use of silica gel adsorption chromatography for the pre-HPLC cleanup step. The schematic shows that (A) a large part of the co-extractives can be removed in the first fraction from the precolumn, (B) the polarity of the mobile phase can be adjusted so the pesticide elutes in pre-HPLC column fraction B where the eluate can be collected and concentrated for injection into the HPLC, while (C) more polar compounds that would otherwise appear during HPLC have been eliminated by permanent adsorption on the pre-HPLC Column. 

The preparation of seawater extracts is described in Chapters 18 and 22. If large amounts of interfering compounds such as biogenic lipids are present in the extracts a pre-clean-up by silica gel adsorption chromatography is recommended (see Chapter 19). 

FIGURE 4.24 Adsorption chromatography of small molecules with a TSK-GEL G2500PWxl column. Column TSK-GEL G2500PWxl, 6 /tm, 7.8 mm X 30 cm. Sample (I) phenylacetic acid. (2) 3-phenylpropionic acid, (3) 4-phenylbutyric acid, (4) benzylamine, (5) 2-phenylethylamine, (6) 3-phenylpropylamine, (7) benzyl alcohol, (8) 2-phenylethanol, and (9) 3-phenyl-1 -propanol. Elution 0.1 M NaCIO, in water. Flow rate 2.0 ml/min. Temperature 65 C. Detection UV at 215 nm. 

Liquid-solid chromatography (LSC). This process, often termed adsorption chromatography, is based on interactions between the solute and fixed active sites on a finely divided solid adsorbent used as the stationary phase. The adsorbent, which may be packed in a column or spread on a plate, is generally a high surface area, active solid such as alumina, charcoal or silica gel, the last... 

In adsorption chromatography, the bed has special characteristics to adsorb solutes. The recommended beds for adsorption chromatography are silica gel, alumina and charcoal. 

Separation by adsorption chromatography takes place preferentially as a result of hydrogen bonding or dipole-dipole interactions. Hence, separation of mixtures of substances on silica gel layers by lipophilic solvents primarily takes place according to polarity differences. Further separation within a polarity group can then be achieved either two-dimensionally or off-line by partition chromatography on anotho TLC plate (Fig. 4). 

Chapter 3 through Chapter 8 deal with the basic aspects of the practical uses of PLC. Chapter 3 describes sorbent materials and precoated layers for normal or straight phase (adsorption) chromatography (silica gel and aluminum oxide 60) and partition chromatography (silica gel, aluminum oxide 150, and cellulose), and precoated layers for reversed-phase chromatography (RP-18 or C-18). Properties of the bulk sorbents and precoated layers, a survey of commercial products, and examples of substance classes that can be separated are given. 

Aluminum oxides, similar to silica gels, are available as bulk materials and as precoated plates, to be used not only for straight phase adsorption chromatography, but also for partition PLC (see Table 3.3 and Table 3.4). In particular, the aluminum oxide type 150 (i.e., mean pore diameter 150 A [15 tun]) is suitable for partition chromatographic purposes. 

For multi-analyte and/or multi-matrix methods, it is not possible to validate a method for all combinations of analyte, concentration and type of sample matrix that may be encountered in subsequent use of the method. On the other hand, the standards EN1528 andEN 12393 consist of a range of old multi-residue methods. The working principles of these methods are accepted not only in Europe, but all over the world. Most often these methods are based on extractions with acetone, acetonitrile, ethyl acetate or n-hexane. Subsequent cleanup steps are based on solvent partition steps and size exclusion or adsorption chromatography on Florisil, silica gel or alumina. Each solvent and each cleanup step has been successfully applied to hundreds of pesticides and tested in countless method validation studies. The selectivity and sensitivity of GC combined with electron capture, nitrogen-phosphorus, flame photometric or mass spectrometric detectors for a large number of pesticides are acceptable. 

Restricted access phases are another approach to exploiting the differences in characteristics of analytes. Large analytes are excluded from an internal surface on which an adsorptive stationary phase is present. A herbicide analysis for Metsulfuron methyl, Bentazone, Bromoxynil, methylchlorophenoxy acid, and Mecoprop in the presence of humic acid was performed on restricted access reversed phase media.52 The cytostatic compound epirubicin and its metabolites were separated from plasma using a Pinkerton GFF II column.53 Gradient separations of polymers on reversed phase and on normal phase represent an alternative to gel permeation chromatography. Polyesters of noncrystalline materials were separated on a variety of such phases.54... 

Fractionation of the oils The oils were fractionated by adsorption chromatography on silica gel. The column was eluted successively with 40 - 60°C petroleum ether (12 fractions),... 

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