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Soxhlet Extraction of Lipid Biomarkers from Sediment

Overview

Source: Laboratory of Jeff Salacup - University of Massachusetts Amherst

Every lab needs standards that track the performance, accuracy, and precision of its instruments over time to ensure a measurement made today is the same as a measurement made a year from now (Figure 1). Because standards must test the performance of instruments over a long period of time, large volumes of the standards are often required. Many chemical standards can be purchased from retail scientific companies, like Sigma-Aldrich and Fisher. However, some compounds that occur in nature and that are relevant to paleoclimatic studies have not yet been isolated and purified for purchase. Therefore, these compounds need to be extracted from natural samples, and because of the large volumes of standards required, large volumes of sediment need to be extracted. The Accelerated Solvent Extraction (Dionex) and sonication extractions are not appropriate for the extraction of such large sediment volumes. In these circumstances, a Soxhlet extraction is used.

Figure 1
Figure 1. Schematic depicting how chemical standard tracks the performance of an instrument through time. The dashed line represents a 1:1 relationship between the accepted and measured (on the instrument) value of a variable. Each star is a weekly measurement of the chemical standard. Green stars represent standards that are accurate. Red stars reflect those that are not accurate indicating that the instrument requires corrective maintenance.

Procedure

1. Setup and Preparation of Materials

  1. Collect a sample of frozen, freeze-dried, crushed, and homogenized marine sediment. A sample like this contains many of the compounds needed for standards.
    1. Standards are often made from sediments that are left over after a coring expedition or analysis. For example, in this experiment, sediment that was obtained from the 'Mud Patch' located just south of Cape Cod is extracted. This sediment was taken as part of a coring expedition but will not be used

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Results

At the end of extraction, a total lipid extract (TLE) for the sample is produced. The round-bottomed flask contains the extractable organic matter from the sediment sample. This TLE can now be analyzed, and its chemical constituents identified and quantified.

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Application and Summary

The extract from the marine mud contains compounds called alkenones, which are used in paleoceanography. Alkenones are long-chained alkyl-ketones produced by certain classes of haptophyte algae that live in the sunlit surface ocean3 (Figure 3). The two most common alkenones are 37 carbon atoms long and have two or three double bonds in them. The haptophytes adjust the ratio of these two alkenones in their cells according to the temperature of the water they live in. The ratio of the two a

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References
  1. Jensen, W. B. The Origin of the Soxhlet Extractor J Chem Ed. 84, 1913-1914, (2007).
  2. Levey, M. Chemistry and Technology in Ancient Mesopotamia, Elsevier. 33-34, (1959).
  3. Conte, M. H., Thompson, A., Eglinton, G. Primary production of lipid biomarker compounds by Emiliania huxleyi: results from an experimental mesocosm study in fjords of southern Norway, Sarsia79, 319-332 (1994).
  4. Brassell, S. C., Eglinton, G., Marlowe, I. T., Pflaumann, U., Sarnthein, M. Molecular Stratigraphy - a New Tool for Climatic Assessment, Nature320 (6058), 129-133 (1986).
  5. Herbert, T. D. Alkenone paleotemperature determinations, in Treatise in Marine Geochemistry, edited by H. Elderfield, Elsevier 391-432 (2003).
  6. Prahl, F. G., Wakeham S. G., Calibration of Unsaturation Patterns in Long-Chain Ketone Compositions for Paleotemperature Assessment, Nature330(6146), 367-369 (1987).
  7. Prahl, F. G., Muehlhausen, L. A., Zahnle, D. L. Further evaluation of long-chain alkenones as indicators of paleoceanographic conditions, Geochimica et Cosmochimica Acta52(9), 2303-2310 (1988).
  8. Müller, P. J. et al. Calibration of the alkenone paleotemperature index U37K′ based on core-tops from the eastern South Atlantic and the global ocean (60°N-60°S), Geochimica et Cosmochimica Acta62(10), 1757-1772 (1998).
  9. Marlowe, I. T. et al. Long-chain Alkenones and Alkyl Alkenoates and the Fossil Coccolith Record of Marine-sediments, Chem Geol88(3-4), 349-375 (1990).
Tags
Soxhlet ExtractionLipid BiomarkersSedimentSolid MaterialSolventCompoundsPaleoclimatic StudiesStandardsInstrument PerformanceBiomarkerStandard PreparationSediment ExtractionFranz Von SoxhletAutomated ExtractionBatch ExtractionEfficiencyVideo TutorialMarine SedimentPaleothermometryEarth ScienceChemistryAssemblyRound bottomed FlaskCold Water CondenserThimbleRefluxingDistillation Path

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Overview

1:16

Principles of Soxhlet Extraction

2:44

Sediment Sample and Extraction Preparation

3:49

Soxhlet Extraction

5:54

Applications

7:36

Summary

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