3.2 Basic principles of supercritical fluid chromatography and  (Page 5/6)

Complicated mixtures containing many components should be subject to an extraction process before they are separated via chromatography. An ideal extraction procedure should be fast, simple, and inexpensive. In addition, sample loss or decomposition should not be experienced at the end of the extraction. Following extraction, there should be a quantitative collection of each component. Ideally, the amount of unwanted materials coming from the extraction should be kept to a minimum and be easily disposable; the waste should not be harmful for environment. Unfortunately, traditional extraction methods often do not meet these requirements. In this regard, SFE has several advantages in comparison with traditional techniques.

The extraction speed is dependent on the viscosity and diffusivity of the mobile phase. With a low viscosity and high diffusivity, the component which is to be extracted can pass through the mobile phase easily. The higher diffusivity and lower viscosity of supercritical fluids, as compared to regular extraction liquids, help the components to be extracted faster than other techniques. Thus, an extraction process can take just 10-60 minutes with SFE, while it would take hours or even days with classical methods.

The dissolving efficiency of a supercritical fluid can be altered by temperature and pressure. In contrast, liquids are not affected by temperature and pressure changes as much. Therefore, SFE has the potential to be optimized to provide a better dissolving capacity.

In classical methods, heating is required to get rid of the extraction liquid. However, this step causes the temperature-sensitive materials to decompose. For SFE, when the critical pressure is removed, a supercritical fluid transforms to gas phase. Because supercritical fluid solvents are chemically inert, harmless and inexpensive; they can be released to atmosphere without leaving any waste. Through this, extracted components can be obtained much more easily and sample loss is minimized.

Instrumentation for sfe

The necessary apparatus for a SFE setup is simple. [link] depicts the basic elements of a SFE instrument, which is composed of a reservoir of supercritical fluid, a pressure tuning injection unit, two pumps (to take the components in the mobile phase in and to send them out of the extraction cell), and a collection chamber.

There are two principle modes to run the instrument:

• Static extraction.
• Dynamic extraction.

In dynamic extraction, the second pump sending the materials out to the collection chamber is always open during the extraction process. Thus, the mobile phase reaches the extraction cell and extracts components in order to take them out consistently.

In the static extraction experiment, there are two distinct steps in the process:

1. The mobile phase fills the extraction cell and interacts with the sample.
2. The second pump is opened and the extracted substances are taken out at once.

In order to choose the mobile phase for SFE, parameters taken into consideration include the polarity and solubility of the samples in the mobile phase. Carbon dioxide is the most common mobile phase for SFE. It has a capability to dissolve non-polar materials like alkanes. For semi-polar compounds (such as polycyclic aromatic hydrocarbons, aldehydes, esters, alcohols, etc.) carbon dioxide can be used as a single component mobile phase. However, for compounds which have polar characteristic, supercritical carbon dioxide must be modified by addition of polar solvents like methanol (CH ³ OH). These extra solvents can be introduced into the system through a separate injection pump.