The Investigation of Lipids in Organic Residues by Gas Chromatography / Mass Spectrometry: Applications to Palaeodietary Studies

  • P. H. Bethell
  • R. P. Evershed
  • L. J. Goad


The use of organic material for dating purposes is well known (Aitken 1990). In the conservation field, artefacts have been analysed for identification purposes for many years (e.g. Mills and White 1987). In the case of archaeological soils, total soil organic matter has been routinely measured (Courty et aI. 1989), as have organic complexes of phosphorus (as part of total soil phosphorus assays) (Bethell and Máté 1989). In the field of palaeodietary studies, emphasis has been placed on the measurement of stable isotopes of carbon and nitrogen, rather than on the identification of actual compounds containing these elements (e.g. DeNiro 1987). In addition, collagen, protein and amino acids from bone have been investigated (e.g. Dennison 1980). The limitations of such work in the past have been largely of a technical nature, and recovery and analysis of intact organic molecules from most archaeological materials was extremely expensive and time consuming. However, aided by technological advances over the last 20 years or so, it is now possible to routinely extract trace quantities of organic natural products from aged material recovered from a variety of archaeological sources.


Bile Acid Plant Sterol Deoxycholic Acid Archaeological Material Faecal Marker 
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  1. Aitken MJ (1990) Science-based dating in archaeology. Longman, London New York (Archaeology Series )Google Scholar
  2. Bell GH, Davidson JN, Emslie-Smith D (1972) Textbook of physiology and biochemistry, 7th edn. Churchill Livingstone, Edinburgh.Google Scholar
  3. Bethell PH, Maté I (1989) The use of soil phosphate analysis in archaeology: A critique. In: Henderson J (ed) Scientific analysis in archaeology, and its interpretation. Oxford University Committee for Archaeology/ UCLA Institute of Archaeology, Oxford, pp 1–29Google Scholar
  4. Bhattacharyya AM (1981) Uptake and esterification of plant sterols by rat small intestine. Am J Physiol 240: G50–55Google Scholar
  5. Björkheim I, Gustafsson JA (1971) Mechanism of microbial transformation of cholesterol into coprostanol. Eur J Biochem 21: 428–432CrossRefGoogle Scholar
  6. Brown RC, Wade TL (1984) Sedimentary coprostanol and hydrocarbon distribution adjacent to a sewage outfall. Water Res 18: 631–632Google Scholar
  7. Chapman JR (1985) Practical organic mass spectrometry. Wiley, ChichesterGoogle Scholar
  8. Christie WW (1989) Gas chromatography and lipids - a practical guide. Oily Press, AyrGoogle Scholar
  9. Condamin J, Formenti F, Metais MO, Michel M, Blond P (1976) The application of gas chromatography to the tracing of oil in ancient amphorae. Archaeometry 18: 195–201CrossRefGoogle Scholar
  10. Courty MA, Goldberg P, Macphail R (1989) Soils and micromorphology in archaeology. Cambridge University Press, CambridgeGoogle Scholar
  11. Custer JF, Ilgenfritz J, Doms KR (1988) A cautionary note on the use of Chemstrips for detection of blood residues on prehistoric stone tools. J Archaeol Sci 15: 343–346CrossRefGoogle Scholar
  12. den Dooren de Jong LE (1961) On the formation of adipocere from fats. Antonie Leuwenhoek J Microbiol Serol 27: 337–361CrossRefGoogle Scholar
  13. DeNiro M (1987) Stable isotopy and archaeology. Am Sci 75: 182–191Google Scholar
  14. Dennison KJ (1980) Amino acids in archaeological bone. J Archaeol Sci 7: 81–86CrossRefGoogle Scholar
  15. Dreyfus JC (1989) L’archéologie moléculaire. Med Sci 5 (8): 607–608Google Scholar
  16. Eglinton G, Curry GB (eds) (1991) Molecules through time: Fossil molecules and biochemical systematics. Royal Society, LondonGoogle Scholar
  17. Eglinton G, Logan GA (1991) Molecular preservation. Philos Trans R Soc Lond B 333: 315–328CrossRefGoogle Scholar
  18. Eglinton G, Maxwell JR, Evershed RP, Barwise AJG (1985) red pigments in petroleum exploration. Interdiscip Sci Rev 10 31: 222–236Google Scholar
  19. Evershed RP (1990) Lipids from samples of skin from seven Dutch bog bodies: A preliminary report. Archaeometry 32 (2): 139–153CrossRefGoogle Scholar
  20. Evershed RP (1993a) Gas chromatography of lipids. In: Hamilton RJ (ed) Lipid analysis: A practical approach, chap 4. Oxford University Press, Oxford, pp. 113–151Google Scholar
  21. Evershed RP (1993b) Mass spectrometry of lipids. In: Hamilton R.J. (ed) Lipid analysis: A practical approach, chap 8. Oxford University Press, Oxford, pp. 263–308Google Scholar
  22. Evershed RP, Connolly RC (1988) Lipid preservation in Lindow Man. Naturwissenschaften 75: 143–145CrossRefGoogle Scholar
  23. Evershed RP, Jerman K, Eglinton G (1985) Pine wood origin for pitch from the Mary Rose. Nature 314 (6011): 528–530CrossRefGoogle Scholar
  24. Evershed RP, Heron CP, Goad LJ (1990) Analysis of organic residues of archaeological origin by high temperature gas chromatography and gas chromatography-mass spectrometry. Analyst 115: 1339–1342CrossRefGoogle Scholar
  25. Evershed RP, Heron CP, Goad LJ (1991) Epicuticular wax components preserved in potsherds as chemical indicators of leafy vegetables in ancient diets. Antiquity 65: 540–544Google Scholar
  26. Evershed RP, Heron CP, Charters S, Goad LJ (1992) The survival of food residues: New methods of analysis, interpretation and application. Proc Br Acad 77: 187–208Google Scholar
  27. Frazer AC (1946) The adsorption of trigyceride fat from the intestine. Physic)! Rev 26: 103–119Google Scholar
  28. Fry GF (1985) Analysis of fecal material. In: Gilbert RI, Mielke JH (eds) The analysis of prehistoric diets. Academic Press, London,pp 127–148Google Scholar
  29. Grimait JO, Fernandez P, Bayona JM, Albaiges J (1990) Assessment of fecal sterols and ketones as indicators of urban sewage inputs to coastal waters. Environ Sci Technol 221- (3): 357–363Google Scholar
  30. Gülaçar FO, Susini A, Klohn M (1990) Preservation and post-mortem transformations of lipids in samples from a 4000-year-old Nubian mummy. J Archaeol Sci 17: 691–705CrossRefGoogle Scholar
  31. Hagelberg E, Sykes B, and Hedges REM (1989) Ancient bone DNA amplified. Nature 342: 485CrossRefGoogle Scholar
  32. Hagelberg E, Bell LS, Allen T, Boyde A, Jones SJ, Clegg JB (1991) Analysis of ancient bone DNA: techniques and applications. Philos Trans R Soc Lond B 333: 399–408CrossRefGoogle Scholar
  33. Haslewood GAD (1967) Bile salts. Methuen, LondonGoogle Scholar
  34. Hatcher PG, McGillivray PA (1979) Sewage contamination in the New YorkGoogle Scholar
  35. Bight: coprostanol as an indicator. Environ Sci Technol 13:1225–1229Google Scholar
  36. Hatcher PG, Keister LE, McGillivray PA (1977) Sterols as sewage specific indicators in New York Bight sediments. Bull Environ Contam Toxicol 17: 491–498Google Scholar
  37. Heizer RF, Napton LK (1969) Biological and cultural evidence from prehistoric human coprolites. Science 165: 563–568CrossRefGoogle Scholar
  38. Heron CP, Evershed RP, Goad LJ (1991) Effects of migration of soil lipids on organic residues associated with buried potsherds. J Archaeol Sci 18: 641–659CrossRefGoogle Scholar
  39. Hohn ME, Meinschein WG (1977) Fatty acids in fossil fruits. Geochim Cosmochim Acta 41: 189–193CrossRefGoogle Scholar
  40. Huang WY, Meinschein WG (1979) Sterols as ecological indicators. Geochim Cosmochim Acta 43: 739–745CrossRefGoogle Scholar
  41. Jennings W (1987) Analytical gas chromatography. Academic Press, LondonGoogle Scholar
  42. Knights BA, Dickson CA, Dickson JH, Breeze DJ (1983) Evidence concerning the Roman military diet at Bearsden, Scotland, in the 2nd century AD. J Archaeol Sci 10: 139–152CrossRefGoogle Scholar
  43. Kuksis A, Child P, Myher JJ, Marai L, Yousef IM, Lewin PK (1978) Bile acids of a 3200-year-old Egyptian mummy. Can J Biochem 56: 1141–1148CrossRefGoogle Scholar
  44. Lin DS, Connor WE, Napton LK, Heizer RF (1978) The steroids of 2000year-old human coprolites. J Lipid Res 19: 215–221Google Scholar
  45. Loy TH, Wood AR (1989) Blood residue analysis at Çayönü Tepesi, Turkey. J Field Archaeol 16: 451–460Google Scholar
  46. Mackenzie AS, Brassell SC, Eglinton G, Maxwell JR (1982) Chemical fossils: The geological fate of steroids. Science 217: 491–504Google Scholar
  47. Martin WJ, Ravi Subbiah MT, Koltke BA, Bark CC, Naylor MC (1973)Google Scholar
  48. Nature of faecal sterols and intestinal bacterial flora. Lipids 8:208–215Google Scholar
  49. Mills JS, White R (1987) The organic chemistry of museum objects. Butterworths, LondonGoogle Scholar
  50. Mills JS, White R (1989) The identity of the resins from the late Bronze age shipwreck at Ulu Burun ( Kas ). Archaeometry 31: 37–44Google Scholar
  51. Muller G, Kanazawa A, Teshima S, (1979) Sedimentary record of fecal pollution in part of Lake Constance by coprostanol determination. Naturwissenschaften 66: 520–521CrossRefGoogle Scholar
  52. Nair PP, Kritchevsky D (eds) (1971) The bile acids: Chemistry, physiology, and metabolism, vol 1: Chemistry. Plenum Press, New YorkGoogle Scholar
  53. Nes WR, Nes WD (1980) Lipids in evolution. Plenum Press, New YorkCrossRefGoogle Scholar
  54. Nishimura M, Koyama T (1977) The occurrence of stanols in various living organisms and the behaviour of sterols in contemporary sediments. Geochim Cosmochim Acta 41: 379–385CrossRefGoogle Scholar
  55. Oudemans TFM, Boon JJ (1 991) Molecular archaeology: Analysis of charred (food) remains from prehistoric pottery by pyrolysis-gas chromatography/mass spectrometry. J Anal Appl Pyrolysis 20: 197–227Google Scholar
  56. Owen RW, Henly PJ, Day DW, Thompson MH, Hill MJ (1985) Fecal steroids and colorectal cancer: Bile acid profiles in low and high risk groups. In: Joossens JV et al. (eds) Diet and human carcinogenesis. Elsevier, Amsterdam, pp 165–170Google Scholar
  57. Pääbo S (1989) Ancient DNA: Extraction, characterisation, molecular cloning, and enzymatic amplification. Proc Natl Acad Sci USA 86: 1939–1943CrossRefGoogle Scholar
  58. Pääbo S, Higuchi RG, Wilson AC (1 988) Mitochondria) DNA sequences from a 7,000-year-old brain. Nucleic Acids Res 16: 9775–9787Google Scholar
  59. Pepe C, Dizabo P (1990) Étude d’une fosse du 13éme siécle par les marqueurs biogeochimiques: Chantier archéologique du Louvre ( Paris ). Rev Archéometrie 14: 23–28Google Scholar
  60. Pepe C, Dizabo P, Scribe P, Dagaux J, Filiaux J, Saliot A (1989) Les marqueurs biogeochimiques: Application a l’archéologie. Rev Archéometrie 13: 1–11Google Scholar
  61. Readman JW, Preston MR, Mantoura RFC (1986) An integrated technique to quantify sewage, oil and PAH pollution in estuarine and coastal environments. Mar Pollut Bull 17: 298–308CrossRefGoogle Scholar
  62. Robinson N, Evershed, RP, Higgs WJ, Eglinton G (1987) Proof of a pine wood origin for pitch from Tudor (Mary Rose) and Etrurian shipwrecks: Application of analytical organic chemistry in archaeology. Analyst 112: 637–644Google Scholar
  63. Rosenfeld RS, Fukushima DK, Hellman L, Gallagher TF (1954) The transformation of cholesterol to coprostanol. J Biol Chem 211: 301–311Google Scholar
  64. Rottländer RCA (1990a) Lipid analysis in the identification of vessel contents. MASCA Res Pap Sci Archaeol 7: 37–40Google Scholar
  65. Rottländer RCA (1990b) Die Resultate der modernen Fettanalytik und ihre Anwendung auf die prähistorischer Forschung. Archaeo-Physika 12: 1354Google Scholar
  66. Rottländer RCA, Schlichtherle H (1979) Food identification of samples from archaeological sites. Archaeo-Physika 10: 260–267Google Scholar
  67. Setchell KDR, Lawson AM (1989) Bile acids. In: Lawson AM (ed) Mass spectrometry. De Gruyter, Berlin, pp 54–125Google Scholar
  68. Setchell KDR, Lawson AM, Tanima N, Sjövall J (1983) General methods for the analysis of metabolic profiles of bile acids and related compounds in feces. J Lipid Res 24: 1085–1100Google Scholar
  69. Szczepanik-van Leeuwen PA, Stellaard F (1979) Detection of atypical bile acids in disease states and their identification by gas chromatography–mass spectrometry–computer techniques. In: Paumgartner G, Stiehl A, Gerok W (eds) Biological effects of bile acids. Proc of Falk Symp 24. MTP Press, Lancaster, pp 287–298Google Scholar
  70. Van Vleet ES, Quinn JG (1979) Early diagenesis of fatty acids and isoprenoid alcohols in estuarine and coastal sediments. Geochim Cosmochim Acta 43: 289–303CrossRefGoogle Scholar
  71. Wales S, Evans J, Leeds AR (1991) The survival of waxes in coprolites: the archaeological potential. In: Budd P, Chapman C, Jackson C, Janaway R, Ottaway B (eds) Archaeological sciences 1989 Proc conf on the application of scientific techniques to archaeology, Bradford, September 1989. Oxbow, Oxford (Oxbow Monograph 9 )Google Scholar
  72. Wyckoff RWG (1972) The biochemistry of animal fossils. Scientechnica, LondonGoogle Scholar

Copyright information

© Springer-Verlag Berlin Heidelberg 1993

Authors and Affiliations

  • P. H. Bethell
  • R. P. Evershed
    • 1
  • L. J. Goad
  1. 1.Department of BiochemistryUniversity of LiverpoolLiverpoolUK

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