Chem3010 Assignments: Chromatography Done by: Claudia Matheson ID number: 620042894 Solid Phase Extraction vs.

Solid Phase Micro extraction Solid Phase Extraction (SPE) and Solid Phase Micro-Extraction (SPME) are separation techniques used to separate analytes from complex matrix samples []. SPE is similar to LiquidLiquid Extraction (LLE), in that it involves a portioning of solutes between two phases []. However, in SPE, a solid stationary phase coated with sorbent materials is used along with a liquid mobile phase. In Solid Phase Extraction (SPE) a sample is loaded onto a conditioned stationary phase where it is washed with an aqueous or buffer solution. These solutions allow for the inferring components or analyte (depending on their affinity to the stationary phase) of the sample to be eluted first. The retained component would then be eluted by an organic mobile phase. Though SPE utilizes both a mobile and stationary phase, in Solid Phase Micro-Extraction (SPME) only a stationary phase is used []. This stationary phase is directly injected into the sample (can be volatile or non-volatile) and permits for the adsorption of the analyte to its surfaces. This occurs until equilibrium is reached. The analyte would then be desorbed when introduced into Gas Chromatography column or High Pressure Liquid Chromatography column. Components of the SPE and SPME both differ in appearances as well as operation. Components of the SPE include a syringe barrel column made from either plastic or glass material. The column normally has a fit positioned above and below the stationary phase along with a stop cock. This stopcock allows for the adjustment of the flow rate. A cartridge or disk is used in the extraction process which may or may not contain a polymeric membrane. However, in SPME the only component used is the silica microfiber. This can either be coated with a polymer or a sorbent which is held in a plunger. Even though SPE and SPME are ideal separation methods there are several advantages and disadvantages associated with both techniques. An advantage of using SPE is the small amount of solvent (mobile phase) used to elude the analyte; whereas no solvent is used in the

Solid Phase Micro-extraction method. Also, SPE enables for a cleaner extract and it has a high recovery for polar compounds. Drawbacks include low recovery of analyte (low precision) and its expensive operation. Advantages associated with SPME consist of its simple operation; low analyte sample can be used and it is convenient. However one setback includes the silica fibers high selectivity. Both SPE and SPME have been used over the past several years in scientific research. They have been improved for intricate chemical analysis by using additional instrumentation such as molecular spectroscopy. In the journal of chromatography A, S.B Junior along with several authors used solid phase micro extraction to extract volatile compounds from chili pepper. In this journal article several different microfibers were used to extract various compounds of the sample. This was then injected into a GC column with a split less injector at a flow rate of 1ml min-1 .The compounds were separated with a hydrogen mobile phase and further analyses were done by a Gas Chromatography-Mass Spectroscopy. Esters were the largest components found. In the article entitled Simultaneous determination of 15 amino glycoside(s) residues in animal derived foods by automated solid-phase extraction and liquid chromatographytandem mass spectrometry Yanfei Toa used automated SPE to extract amino glycoside from animal liver. Carbolic acid cartridges were used in this analysis and the flow rate was 10ml/min.

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