Modern Techniques for the Extraction of Solid Materials — An Update - - Chromatography Online
Modern Techniques for the Extraction of Solid Materials — An Update


LCGC Asia Pacific
Volume 9, Issue 3


Ronald E. Majors
In June 1999, LCGC published a special supplement that focused on the sample preparation of solids (1). At that time, we covered general methods — supercritical fluid extraction (SFE), pressurized fluid extraction–accelerated solvent extraction (PFE–ASE), microwave-assisted extraction (MAE), and automated Soxhlet extraction. In the ensuing six years, these modern extraction techniques have continued to evolve. In some cases, systems have been further miniaturized and automated. A wider variety of applications has been achieved in such diverse areas as environmental, pharmaceutical, natural product, food, and polymer chemistry. In this installment of "Sample Preparation Perspectives," I will update the earlier coverage and make a note of some of the instrumental advances and a few applications that have spurred the growth of these extraction techniques. Although the literature abounds with applications examples, this review will focus on the technology. Websites of the various manufacturers, textbooks, and review articles are great sources of information on applications examples.




Modern liquid–solid extraction has its roots in the shake–filter method. Basically, the shake–filter extraction method involves the intimate contact between a solid material, usually finely divided, and a solvent that has an optimum solubility for the analyte of interest and a minimum solubility for the matrix. The technique works well for porous matrices where the solvent can diffuse into the pores and extract analytes. Sometimes mechanical agitation and heating is used to speed up the extraction process. At the conclusion of the experiment, insoluble materials are removed by filtration or centrifugation. For some samples, the extract can immediately be injected into a chromatograph for further separation. More often, there is some additional sample preparation required to isolate the critical analytes from other extractables that can interfere with the chromatography step.

For more intimate contact between solvent, the adsorbed (absorbed) analyte and matrix, other sample preparation techniques might be required. Several methods that can achieve this intimate contact include homogenization, sonication, emulsification, or vortexing. For biological samples, various cell disruption techniques can be employed. All of these methods require the application of an additional external force (or forces) to the sample in suspension.


Table I: Most modern solid extraction techniques use increased temperature and pressure
Most modern liquid–solid extraction techniques use increased temperature or pressure to increase the rate of extraction. Table I summarizes the influence of these parameters on analyte extraction.

Modern Soxhlet Extraction

Soxhlet extraction is by far the most widely used method for solid sample pretreatment. In fact, it is the de facto standard with which all other extraction procedures are compared and contrasted. Soxhlet extraction is simple, effective, and relatively inexpensive. Generally, it provides good analyte recovery but its traditional operation is slow and uses copious amounts of solvent. Although classical Soxhlet extractions can last as long as 18–24 h, once set up and running, the experiment requires very little user involvement. Small-volume Soxhlet systems are available, but the sample size often is dictated by the analyte concentration, the necessary mass to obtain a representative sample, and the chromatography detector sensitivity, all of which could combine to require a larger sample size.


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