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Solid-phase extraction: principles, techniques, and by Nigel J.K. Simpson

By Nigel J.K. Simpson

Reference and textual content demonstrates the connection of the elemental conception of solid-phase extraction (SPE) to chromatography, illustrating how SPE strategies considerably give a contribution to the practise of samples for a wide selection of analytical innovations.

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The bonded organic group is somewhat mobile except for the attachment at one end. For a small R group the movement is Restricted access to residual very restricted so access to silanols on either polymeric or the nearby surface (silanols) monomeric ~ h a s e s R R is not hindered to any extent. ---'/ OH 0 I I \ /ii O 0 /ii\o ; O I ox I \ , f / i i, \ /ji O o O O O O O X = H or Si (OX),R Figure 6. Illustration of the blocking effect of neighboring bonded-phase groups on adjacent silanols. Copyright © 2000 by Taylor & Francis Group LLC However if R is large like octadecyl (C-18), then the movement of the alkyl chain prevents other organic moieties from reaching the surface, particularly if they are large also.

Sample additives that release a non-polar drug by making it more soluble in the liquid phase of a sample also reduce the strength of retention on a nonpolar sorbent. One possible approach to elimination of protein binding may be drawn by analogy to biochemical receptor inhibition. By adding to the sample an excess of a compound which competitively displaces the analyte from the binding sites on the protein, the effect of the protein on extraction efficiency should be reduced. The difficulty with this approach is that the nature of the analytelprotein interaction must be accurately known or estimated and the added compound must not interfere with the extraction or analysis.

Filter homogenate 2. Dilute 5: 1 with water/l% AcOH 3. MeOH and waterll% AcOH conditioning 4. Apply sample 5. 1M K,HPO, 6. 1M K,HPO, 1: 1 (vlv) 1. Dilute corn oil 1: 10 with hexane 2. Hexane conditioning 3. Apply sample 4. Wash with 1 mL hexane 5. Elute with 1 mL MeOH Atrazine has a solubility in pure water of 70 ppm (parts per million) at 25°C. In a seawater sample at ambient temperature this solubility is expected to be lower still. Thus, atrazine is unlikely to be found in excess of a maximum concentration of a few micrograms per milliliter.

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