Characterization of selected immobilized metal-ions using solid phase extraction sorbents

摘要

Solid phase extraction (SPE) has been developed as an alternative to liquid-liquid extraction (LLE) in the sample preparation process. The advantages of SPE over LLE are that it is a more useful, reliable tool for sample preparation, which offers greater selectivity. The selectivity of an SPE sorbent is vital for the isolation of analyte from a biological matrix containing a myriad of interferences. The use of conventional ion exchange SPE for such an extraction process might not be adequate due to the adverse effects of interfering ions. Metals immobilized on various modified silicas were investigated to determine if the addition of metals improved selectivity. The selectivity of these sorbents was studied by the extraction of analytes from high ionic strength matrices. Extraction selectivity was found to depend on different factors, including the type of bonded species, metal ions used and the analytes, counter ions, sample pH and elution solvent composition. Utilizing coordination complexation between analytes and immobilized metal ions, particularly when different phases are stacked, can increase selectivity for a particular analyte. Metals immobilized by ionic exchange sorbents were observed to retain analytes of tridentate chelation capability more than immobilized metals on bonded chelators. However, bonded chelators were observed to be advantageous because they more strongly retained metal ions, relative to ionic exchangers. The interactions of immobilized silver ions with unsaturated molecules utilizing SPE were investigated. Retention of silver ions was found dependent on the nature of bonded phase. The silver ions immobilized by coordination interactions showed weaker retention than silver immobilized by ionic interactions. Retention of alkenes by silver was found to have higher flow dependence, as compared to ionic exchange or ligand exchange processes. Retention of analytes was observed to depend on a variety of factors, including the type of bonded phase used for silver immobilization, the composition of the elution solvent, steric factors, the degree of unsaturation, the geometry and position of the double bonds of the analyte molecules. Extraction selectivity for geometrical isomers decreased when silver ions were immobilized by long chain cation exchangers versus those on conventional short chain cation exchangers.