Extraction Technologies for Medicinal and Aromatic ... - Capacity4Dev
Extraction Technologies for Medicinal and Aromatic ... - Capacity4Dev Extraction Technologies for Medicinal and Aromatic ... - Capacity4Dev
9 SOLID PHASE MICRO-EXTRACTION AND HEADSPACE TRAPPING EXTRACTION SPME was introduced in 1990 as a solvent-free sample preparation technique. The basic principal of this approach is to use a small amount of the extracting phase, usually less than 1 microliter. Sample volume can be large when the investigated material is sampled directly, e.g. the air in a room. The extracting phase can be either a high molecular weight polymeric liquid, similar in nature to stationary phases in chromatography, or a solid sorbent, typically of a high porosity, to increase the surface area available for adsorption. The configuration of SPME is a small, fused silica fiber, usually coated with a polymeric phase. The fiber is mounted for protection in syringelike device. The analytes are absorbed or adsorbed by the fiber phase until equilibrium is reached in the system. The amount of an analyte extracted by the coating at equilibrium is determined by the magnitude of the partition coefficient of the analyte between the sample matrix and the coating material. In SPME, analytes typically are not extracted quantitatively from the matrix. Equilibrium methods are more selective because they take full advantage of the difference between extracting phase and matrix distribution constants to separate target analytes from interferences. Exhaustive extraction can be achieved in SPME, and this can be accomplished for most compounds by the application of an internally cooled fi ber. In exhaustive extraction, selectivity is sacrifi ced to obtain quantitative transfer of target analytes to the extracting phase. SPME is ideal for field monitoring. It is unnecessary to measure the volume of the extracted sample, and therefore the SPME device can be exposed directly to the investigated material for quantification of analytes of interest. In addition, extracted analytes are introduced into the instrument by simply placing the fiber in the desorbtion unit. This convenient, solvent-free process results in sharp injection bands and rapid separations. 9.2 The SPME Device The commercial SPME device manufactured by Supelco (Bellefonte, USA) is presented in Figure 1. The fi ber glued into a piece of stainless steel tubing is mounted on a special holder. The holder is equipped with an adjustable depth gauge, which makes it possible to control repeatedly, how far the needle of the device penetrates the sample container or the injector. This is important, as the fi ber can break if it hits an obstacle. The movement of the plunger is limited by a small screw that moves in the z-shaped slot of the device. For protection during storage or septum piercing, the fi ber is withdrawn into the needle of the device, with the screw in the uppermost position. During extraction or desorption, the fi ber is exposed by depressing the plunger. The plunger is moved to its lowermost position only for replacement of the fi ber assembly. Each type of fi ber has a hub of a different color. 146
EXTRACTION TECHNOLOGIES FOR MEDICINAL AND AROMATIC PLANTS Figure 1: The SPME device If the sample is in a vial, the septum of the vial is fi rst pierced with the needle (with the fi ber in the retracted position), and the plunger is lowered, which exposes the fi ber to sample. The analytes are allowed to partition into the coating for a pre-determined time, and the fi ber is then retracted back to the needle. The device is then transferred to the SPME instrument. When gas chromatography is used for analyte separation and quantifi cation, the fi ber is inserted into a hot injector, where thermal desorption of the trapped analyte takes place. For spot sampling, the fi ber is exposed to a sample matrix until partitioning equilibrium is reached between sample matrix and the coating material. In the time average approach, on the other hand, the fi ber remains in the needle during exposure of the SPME device to the sample. The coating works as a trap for the analytes that diffuse into the needle, resulting in integral concentration over time measurements. SPME sampling can be performed in three basic modes: direct extraction, headspace trapping, and extraction with membrane protection. 147
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EXTRACTION TECHNOLOGIES FOR MEDICINAL AND AROMATIC PLANTS<br />
Figure 1: The SPME device<br />
If the sample is in a vial, the septum of the vial is fi rst pierced<br />
with the needle (with the fi ber in the retracted position), <strong>and</strong> the plunger is<br />
lowered, which exposes the fi ber to sample. The analytes are allowed to<br />
partition into the coating <strong>for</strong> a pre-determined time, <strong>and</strong> the fi ber is then<br />
retracted back to the needle. The device is then transferred to the SPME<br />
instrument. When gas chromatography is used <strong>for</strong> analyte separation <strong>and</strong><br />
quantifi cation, the fi ber is inserted into a hot injector, where thermal desorption<br />
of the trapped analyte takes place.<br />
For spot sampling, the fi ber is exposed to a sample matrix until<br />
partitioning equilibrium is reached between sample matrix <strong>and</strong> the coating<br />
material. In the time average approach, on the other h<strong>and</strong>, the fi ber remains<br />
in the needle during exposure of the SPME device to the sample. The coating<br />
works as a trap <strong>for</strong> the analytes that diffuse into the needle, resulting in<br />
integral concentration over time measurements.<br />
SPME sampling can be per<strong>for</strong>med in three basic modes: direct<br />
extraction, headspace trapping, <strong>and</strong> extraction with membrane protection.<br />
147