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Analysis of amino acid 13 C abundance from human and faunal bone collagen using liquid chromatography/isotope ratio mass spectrometry
Author(s) -
McCullagh James S. O.,
Juchelka Dieter,
Hedges Robert E. M.
Publication year - 2006
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.2651
Subject(s) - chemistry , isotope ratio mass spectrometry , chromatography , mass spectrometry , high performance liquid chromatography , amino acid , isotope , hydrolysate , organic chemistry , hydrolysis , biochemistry , quantum mechanics , physics
Abstract The scope of compound‐specific stable isotope analysis has recently been increased with the development of the LC IsoLink which interfaces high‐performance liquid chromatography (HPLC) and isotope ratio mass spectrometry (IRMS) to provide online LC/IRMS. This enables isotopic measurement of non‐volatile compounds previously not amenable to compound‐specific analysis or requiring substantial modification for gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS), which results in reduced precision. Amino acids are an example of such compounds. We present a new chromatographic method for the HPLC separation of underivatized amino acids using an acidic, aqueous mobile phase in conjunction with a mixed‐mode stationary phase that can be interfaced with the LC IsoLink for compound‐specific δ 13 C analysis. The method utilizes a reversed‐phase Primesep‐A column with embedded, ionizable, functional groups providing the capability for ion‐exchange and hydrophobic interactions. Baseline separation of 15 amino acids and their carbon isotope values are reported with an average standard deviation of 0.18‰ (n = 6). In addition δ 13 C values of 18 amino acids are determined from modern protein and archaeological bone collagen hydrolysates, demonstrating the potential of this method for compound‐specific applications in a number of fields including metabolic, ecological and palaeodietary studies. Copyright © 2006 John Wiley & Sons, Ltd.