Bonded phase selection

Ion-exchange solid-phase extractions are used for ionic compounds. The pH of the extracts is adjusted to ionize the target analytes so that they are preferentially retained by the stationary bonded phase. Selection of the bonded phase depends on the pK or pA b of the target analytes. Sample cleanup using ion exchange is highly selective and can separate polar ionic compounds that are difficult to extract by the liquid-liquid partition technique. 

Bonded amine Si-O-Si-C -ch2ch2ch2-nh2 Polar bonded phase Selectivity is modified with respect to silica through the aminopropyl functionality the propyl linkage can interact... 

Some General Guidelines for Bonded Phase Selection 56... 

These aspects of bonded phase selection are, of course, very difficult to assess. However, a brief, necessarily incomplete general guide to this topic can be given. 

D. E. Martire and R. E. Boehm, A unified theory of retention and selectivity in liquid chromatography. 2. Reversed-phase liquid clrromatography with chemically bonded phases , J. Phys. Chem. 87 1045-1062 (1983). 

To retain solutes selectively by dispersive interactions, the stationary phase must contain no polar or ionic substances, but only hydrocarbon-type materials such as the reverse-bonded phases, now so popular in LC. Reiterating the previous argument, to ensure that dispersive selectivity dominates in the stationary phase, and dispersive interactions in the mobile phase are minimized, the mobile phase must now be strongly polar. Hence the use of methanol-water and acetonitrile-water mixtures as mobile phases in reverse-phase chromatography systems. An example of the separation of some antimicrobial agents on Partisil ODS 3, particle diameter 5p is shown in figure 5. 

Many racemic mixtures can be separated by ordinary reverse phase columns by adding a suitable chiral reagent to the mobile phase. If the material is adsorbed strongly on the stationary phase then selectivity will reside in the stationary phase, if the reagent is predominantly in the mobile phase then the chiral selectivity will remain in the mobile phase. Examples of some suitable additives are camphor sulphonic acid (10) and quinine (11). Chiral selectivity can also be achieved by bonding chirally selective compounds to silica in much the same way as a reverse phase. A example of this type of chiral stationary phase is afforded by the cyclodextrins. 

In summary, the development of materials for the extraction of pesticides from water samples has progressed from simple liquid-liquid extraction for the principal active compound to sophisticated SPE media capable of exclusively trapping the target pesticide and metabolites selectively. The development of alkyl bonded phase silica cartridges and extraction disks combined with on-line extraction techniques is currently the principal means used for the extraction and trace enrichment of pesticides and metabolites from water. 

Sllylation, preparation of bonded phases (LC) 324 Simplex optimization selectivity (LC) 478 temperature program (GC) 56 Single column ion chroBatography 434, 438 Sintered glass layer (TLC) 671 Size-exclusion chroBatography 439... 

Figure 4.27 Flow chart for coluwi selection based on sample type (m - molecular weight). PLC precipitation-liquid chromatography SEC = size-exclusion chromatography lEC - ion-exchange chromatography HIC hydrophobic interaction chromatography LSC liquid-solid chromatography RPC - reversed-phase liquid chromatography BPC (polar) bonded-phase chromatography and IPC - ion-pair chromatography.

The PRISMA model was developed by Nyiredy for solvent optimization in TLC and HPLC [142,168-171]. The PRISMA model consists of three parts the selection of the chromatographic system, optimization of the selected mobile phases, and the selection of the development method. Since silica is the most widely used stationary phase in TLC, the optimization procedure always starts with this phase, although the method is equally applicable to all chemically bonded phases in the normal or reversed-phase mode. For the selection of suitable solvents the first experiments are carried out on TLC plates in unsaturated... 

Silica has often been modified with silver for argentation chromatography because of the additional selectivity conferred by the interactions between silver and Jt-bonds of unsaturated hydrocarbons. In a recent example, methyl linoleate was separated from methyl linolenate on silver-modified silica in a dioxane-hexane mixture.23 Bonded phases using amino or cyano groups have proved to be of great utility. In a recent application on a 250 x 1-mm Deltabond (Keystone Scientific Belief onte, PA) Cyano cyanopropyl column, carbon dioxide was dissolved under pressure into the hexane mobile phase, serving to reduce the viscosity from 6.2 to 1 MPa and improve efficiency and peak symmetry.24 It was proposed that the carbon dioxide served to suppress the effect of residual surface silanols on retention. 

Gilpin, R. K., Jaroniec, M., and Lin, S., Dependence of the methylene selectivity on the composition of hydro-organic eluents for reversed-phase liquid chromatographic systems with alkyl bonded phases, Chromatographia, 30,393, 1990. 

Czajowska, T. and Jaroniec, M., Selectivity of alkylamide bonded-phase with respect to organic acids under reversed-phase conditions, J. Chromatogr. A, 762(1 2), 147, 1997. 

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