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Dating Reassembled Collagen from Fossil Bones

Published online by Cambridge University Press:  03 August 2017

Larisa Goldenberg ,
Lior Regev ,
Eugenia Mintz  and
Elisabetta Boaretto
Larisa Goldenberg
Affiliation:
Weizmann Institute of Science, Max Planck-Weizmann Center for Integrative Archaeology and Anthropology, Rehovot, Israel
Lior Regev
Affiliation:
Weizmann Institute of Science, Ringgold Standard Institution, D-REAMS Radiocarbon Laboratory, Max Planck-Weizmann Center for Integrative Archaeology and Anthropology, Rehovot, Israel
Eugenia Mintz
Affiliation:
Weizmann Institute of Science, Scientific Archaeology Unit, Rehovot, Israel
Elisabetta Boaretto*
Affiliation:
Weizmann Institute of Science, Ringgold Standard Institution, D-REAMS Radiocarbon Laboratory, Max Planck-Weizmann Center for Integrative Archaeology and Anthropology, Rehovot, Israel Weizmann Institute of Science, Scientific Archaeology Unit, Rehovot, Israel
*
*Corresponding author. Email: elisabetta.boaretto@weizmann.ac.il.
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Abstract

Insoluble bone collagen is one of the most common materials used for high-resolution radiocarbon (14C) dating. Unfortunately, in some bones, poor preservation of the insoluble collagen excludes the possibility of dating. During the burial of the bone the collagen sometimes degrades into peptides. These peptides are soluble in the acid used to dissolve the bone mineral. It is known that under appropriate conditions, collagen has the ability to self-assemble. Here we exploit this capability and present a method for reassembling the soluble collagen peptides in archaeological bones and dating them. We treated the acid fraction generated during the demineralization of the bone by desalting and neutralizing the solution by dialysis. During the dialysis, the soluble collagen peptides reassemble and precipitate in the dialysis bag. We used FTIR spectroscopy to determine that the precipitated material is indeed collagen. The 14C dates obtained from the reassembled collagen were compared to the dates of “standard” insoluble collagen, extracted in parallel from the same bone. Although there are some divergences of the dates, 3 out of 10 samples could have been dated only by the reassembled collagen. This shows that collagen peptides reassembly can be a valuable tool for dating bones with little or no insoluble collagen.

Keywords

AMS datingcollagencollagen reassemblydegradationFTIR spectroscopy
Type
Method Development
Information
Radiocarbon , Volume 59 , Special Issue 5: 8th International Symposium, Edinburgh, 27 June – 1 July, 2016 Part 1 of 2 , October 2017 , pp. 1487 - 1496
Copyright
© 2017 by the Arizona Board of Regents on behalf of the University of Arizona 

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Footnotes

Selected Papers from the 8th Radiocarbon & Archaeology Symposium, Edinburgh, UK, 27 June–1 July 2016

References

REFERENCES

Ajie, HO, Kaplan, IR, Slota, PJ, Taylor, R. 1990. AMS radiocarbon dating of bone osteocalcin. Nuclear Instruments and Methods in Physics Research B 52(3–4):433–437.Google Scholar
Ambrose, SH, Butler, BM, Hanson, DB, Hunter-Anderson, RL, Krueger, HW. 1997. Stable isotopic analysis of human diet in the Marianas Archipelago, Western Pacific. American Journal of Physical Anthropology 104(3):343–361.Google Scholar
Boaretto, E, Wu, X, Yuan, J, Bar-Yosef, O, Chu, V, Pan, Y, Liu, K, Cohen, D, Jiao, T, Li, S, Gu, H, Goldberg, P, Weiner, S. 2009. Radiocarbon dating of charcoal and bone collagen associated with early pottery at Yuchanyan Cave, Hunan Province, China. Proceedings of the National Academy of Sciences 106(24):9595–9600.CrossRefGoogle ScholarPubMed
Brandt, E, Wiechmann, I, Grupe, G. 2002. How reliable are immunological tools for the detection of ancient proteins in fossil bones? International Journal of Osteoarchaeology 12(5):307–316.CrossRefGoogle Scholar
Brock, F, Geoghegan, V, Thomas, B, Jurkschat, K, Higham, T. 2013. Analysis of bone “collagen” extraction products for radiocarbon dating. Radiocarbon 55(2–3):445–463.CrossRefGoogle Scholar
Brown, TA, Nelson, DE, Vogel, JS, Southon, JR. 1988. Improved collagen extraction by modified Longin method. Radiocarbon 30(2):171–177.Google Scholar
Cherkinsky, A. 2009. Can we get a good radiocarbon age from “bad bone”? Determining the reliability of radiocarbon age from bioapatite. Radiocarbon 51(2):647–655.CrossRefGoogle Scholar
Collins, MJ, Child, AM, Turner, WG. 1995. A basic mathematical similation of the chemical degradation of ancient collagen. Journal of Archaeological Science 22:175–183.CrossRefGoogle Scholar
Collins, MJ, Nielsen-Marsh, CM, Hiller, J, Smith, CI, Roberts, JP, Prigodich, RV, Wess, TJ, Csapó, J, Millard, AR, Turner-Walker, G. 2002a. The survival of organic matter in bone: a review. Archaeometry 44:383–394.CrossRefGoogle Scholar
Collins, MJ, Nielsen-Marsh, CM, Hiller, J, Smith, CI, Roberts, JP, Prigodich, RV, Wess, TJ, Csapò, J, Millard, AR, Turner-Walker, G. 2002b. The survival of organic matter in bone: a review. Archaeometry 44(3):383–394.CrossRefGoogle Scholar
D’Elia, M, Gianfrate, G, Quarta, G, Giotta, L, Giancane, G, Calcagnile, L. 2007. Evaluation of possible contamination sources in the 14C analysis of bone samples by FTIR spectroscopy. Radiocarbon 49(02):201–210.CrossRefGoogle Scholar
De Vries, HL, Barendsen, GW. 1954. Measurements of age by the carbon-14 technique. Nature 174(4442):1138–1141.CrossRefGoogle Scholar
DeNiro, MJ, Weiner, S. 1988. Chemical, enzymatic and spectroscopic characterization of collagen and other organic fractions from prehistoric bones. Geochimica et Cosmochimica Acta 52:2197–2206.CrossRefGoogle Scholar
Elster, H, Gil-Av, E, Weiner, S. 1991. Amino acid racemization of fossil bone. Journal of Archaeological Science 18:605–617.Google Scholar
Fessler, JH. 1974. Self-assembly of collagen. Journal of Supramolecular Structure 2(2–4):99–102.CrossRefGoogle ScholarPubMed
Fraser, RDB, MacRae, TP, Suzuki, E. 1979. Chain conformation in the collagen molecule. Journal of Molecular Biology 129(3):463–481.CrossRefGoogle ScholarPubMed
Gillespie, R. 1989. Fundamentals of bone degradation chemistry: collagen is not “the way”. Radiocarbon 31(3):239–246.Google Scholar
Gross, J, Kirk, D. 1958. The heat precipitation of collagen from neutral salt solutions: some rate-regulating factors. Journal of Biological Chemistry 233(2):355–360.CrossRefGoogle ScholarPubMed
Haas, H, Banewicz, J. 1980. Radiocarbon dating of bone apatite using thermal release of CO2 . Radiocarbon 22(2):537–544.Google Scholar
Haynes, V. 1968. Radiocarbon: analysis of inorganic carbon of fossil bone and enamel. Science 161(3842):687–688.CrossRefGoogle ScholarPubMed
Hedges, REM. 2002. Bone diagenesis: an overview of processes. Archaeometry 44:319–328.CrossRefGoogle Scholar
Hedges, REM, Millard, AR. 1995. Bones and groundwater-towards the modeling of diagenetic processes. Journal of Archaeological Science 22(2):155–164.Google Scholar
Hedges, REM, van Klinken, GJ. 1992. A review of current approaches in the pretreatment of bone for radiocarbon dating by AMS. Radiocarbon 34(2):279–291.Google Scholar
Helseth, DL, Veis, A. 1981. Collagen self-assembly in vitro. Differentiating specific telopeptide–dependent interactions using selective enzyme modification and the addition of free amino telopeptide. Journal of Biological Chemistry 256(14):7118–7128.Google Scholar
Holmes, D, Capaldi, M, Chapman, J. 1986. Reconstitution of collagen fibrils in vitro; the assembly process depends on the initiating procedure. International Journal of Biological Macromolecules 8(3):161–166.Google Scholar
Jans, MME, Nielsen-Marsh, CM, Smith, CI, Collins, MJ, Kars, H. 2004. Characterisation of microbial attack on archaeological bone. Journal of Archaeological Science 31:87–95.Google Scholar
Kadler, KE, Holmes, DF, Trotter, JA, Chapman, JA. 1996. Collagen fibril formation. Biochemical Journal 316(Pt 1):1–11.CrossRefGoogle ScholarPubMed
Katz, EP, Li, S. 1973. Structure and function of bone collagen fibrils. Journal of Molecular Biology 80:1–15.CrossRefGoogle ScholarPubMed
Law, IA, Hedges, R. 1989. A semi-automated bone pretreatment system and the pretreatment of older and contaminated samples. Radiocarbon 31(3):247–253.Google Scholar
Longin, R. 1971. New method of collagen extraction for radiocarbon dating. Nature 230(5291):241–242.Google Scholar
McCullagh, J, Marom, A, Hedges, R. 2010. Radiocarbon dating of individual amino acids from archaeological bone collagen. Radiocarbon 52(2):620–634.CrossRefGoogle Scholar
Otsubo, K, Katz, EP, Mechanic, GL, Yamauchi, M. 1992. Cross-linking connectivity in bone collagen fibrils: the carboxy-terminal locus of free aldehyde. Biochemistry 31(2):396–402.CrossRefGoogle Scholar
Ramachandran, GN, Sasisekharan, V. 1968. Conformation of polypeptides and proteins. In: Anfinsen CB, Frederic MR, editors. Advances in Protein Chemistry. Academic Press. p 283–437.Google Scholar
Richards, MP, Hedges, REM. 1999. Stable isotope evidence for similarities in the types of marine foods used by late Mesolithic humans at sites along the Atlantic coast of Europe. Journal of Archaeological Science 26(6):717–722.CrossRefGoogle Scholar
Sillen, A, Parkington, J. 1996. Diagenesis of bones from Eland’s Bay Cave. Journal of Archaeological Science 23(4):535–542.CrossRefGoogle Scholar
Smith, CI, Nielsen-Marsh, CM, Jans, MME, Collins, MJ. 2007. Bone diagenesis in the European Holocene I: patterns and mechanisms. Journal of Archaeological Science 34(9):1485–1493.Google Scholar
Stafford, TW, Duhamel, RC, Haynes, CV, Brendel, K. 1982. Isolation of proline and hydroxyproline from fossil bone. Life Sciences 31(9):931–938.CrossRefGoogle ScholarPubMed
Stiner, MC, Kuhn, SL, Weiner, S, Bar-Yosef, O. 1995. Differential burning, recrystallization, and fragmentation of archaeological bone. Journal of Archaeological Science 22:223–237.Google Scholar
Stuiver, M, Polach, HA. 1977. Discussion: reporting 14C data. Radiocarbon 19(3):355–363.CrossRefGoogle Scholar
Taylor, RE. 1992. Radiocarbon dating of bone: to collagen and beyond. In: Taylor E, Long A, Kra RS, editors. Radiocarbon After Four Decades: An Interdisciplinary Perspective. New York: Springer. p 375–402.CrossRefGoogle Scholar
Termine, JD. 1988. Non-collagen proteins in bone. Ciba Foundation Symposium 136 – Cell and Molecular Biology of Vertebrate Hard Tissues. John Wiley & Sons, Ltd. p 178–206.Google Scholar
Tuross, N, Stathoplos, L. 1993. Ancient proteins in fossil bones. Methods in Enzymology. Academic Press. p 121–9.CrossRefGoogle Scholar
Van Der Merwe, NJ, Vogel, JC. 1978. 13C content of human collagen as a measure of prehistoric diet in woodland North America. Nature 276(5690):815–816.Google Scholar
Weiner, S. 2010. Microarchaeology: Beyond the Visible Archaeological Record. Cambridge University Press.Google Scholar
Weiner, S, Bar-Yosef, O. 1990. States of preservation of bones from prehistoric sites in the Near East: a survey. Journal Archaeological Science 17:187–196.Google Scholar
Wood, GC. 1960. The formation of fibrils from collagen solutions. 2. A mechanism for collagen-fibril formation. Biochemical Journal 75(3):598–605.CrossRefGoogle ScholarPubMed
Wood, GC, Keech, MK. 1960. The formation of fibrils from collagen solutions 1. The effect of experimental conditions: kinetic and electron–microscope studies. Biochemical Journal 75(3):588–598.Google Scholar
Wright, LE, Schwarcz, HP. 1996. Infrared and isotopic evidence for diagenesis of bone apatite at Dos Pilas, Guatemala: palaeodietary implications. Journal of Archaeological Science 23(6):933–944.Google Scholar
Yizhaq, M, Mintz, G, Cohen, I, Khalally, H, Weiner, S, Boaretto, E. 2005. Quality controlled radiocarbon dating of bones and charcoal from the early Pre-Pottery Neolithic B (PPNB) of Motza (Israel). Radiocarbon 47(2):193–206.CrossRefGoogle Scholar
Zazzo, A, Saliège, JF. 2011. Radiocarbon dating of biological apatites: a review. Palaeogeography, Palaeoclimatology, Palaeoecology 310(1–2):52–61.Google Scholar
Zhu, J, Kaufman Laura, J. 2014. Collagen I self–assembly: revealing the developing structures that generate turbidity. Biophysical Journal 106(8):1822–1831.Google Scholar