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El-Seedi HR, Smet PA, Beck O, Possnert G, Bruhn JG. 
“Prehistoric peyote use: Alkaloid analysis and radiocarbon dating of archaeological specimens of Lophophora from Texas”. 
J Ethnopharmacol. 2005 Oct 3;101(1-3):238-42.
Two archaeological specimens of peyote buttons, i.e. dried tops of the cactus Lophophora williamsii (Lem.) Coulter, from the collection of the Witte Museum in San Antonio, was subjected to radiocarbon dating and alkaloid analysis. The samples were presumably found in Shumla Cave No. 5 on the Rio Grande, Texas. Radiocarbon dating shows that the calibrated 14C age of the weighted mean of the two individual dated samples corresponds to the calendric time interval 3780-3660 BC (one sigma significance). Alkaloid extraction yielded approximately 2% of alkaloids. Analysis with thin-layer chromatography (TLC) and gas chromatography-mass spectrometry (GC-MS) led to the identification of mescaline in both samples. No other peyote alkaloids could be identified. The two peyote samples appear to be the oldest plant drug ever to yield a major bioactive compound upon chemical analysis. The identification of mescaline strengthens the evidence that native North Americans recognized the psychotropic properties of peyote as long as 5700 years ago.
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Apr 17, 2011 1:59
Confirming and Correcting Earlier Finding #

This paper more precisely identifies the date of the two peyote buttons from the Shumla cave number 5 which had been more loosely radio-carbon dated to '7000 years ago'. Peter Furst mentioned that earlier radiocarbon dating in his review of Stewart's 'Peyote Religion: A History', but the only citation was a personal communication. The authors of this paper reproduced these results, dating the peyote to 3700BC and showing 2% remaining alkaloid content with the major alkaloid being mescaline.

As the authors say: 'From a scientific point of view, the now studied 'mescal buttons' appears to be the oldest plant drugs which ever yielded a major bioactive compound upon phytochemical analysis. From a cultural perspective, our identification of mescaline strengthens the evidence that native North Americans already recognized and valued the psychotropic properties of the peyote cactus 5700 years ago.'
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