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                                                   13
                              Table 4.5  Variations of  C-Enrichment Level in Methamphetamine
                              Synthesized with Different Percentage of  C-Methylamine.
                                                                  13
                                                                                Ratio in [C 3 H 8 N] +
                              Sample  Methamphetamine  13 C-Methylamine  13 C to  C  Measured
                                                                           12
                                No.       Yield (%)      Used (%)     Calculated  Average  Std. dev.
                                 7          31.0            0.0        0.03961  0.03873  0.00068
                                 9          22.0            0.0                 0.03944  0.00045
                                14          7.5             0.25       0.04199  0.04140  0.00074
                                16          6.4             0.25                0.04156  0.00071
                                17          58.0            0.25                0.04166  0.00071
                                13          26.0            0.50       0.04439  0.04414  0.00066
                                12          18.0            1.0        0.04932  0.04844  0.00083
                                15          40.0            1.0                 0.04871  0.00103
                                10          31.0            2.0        0.05932  0.05803  0.00096
                                11          23.0            4.0        0.07956  0.07623  0.00143
                              Source: Low, I.A. et al., Gas chromatographic/mass spectrometric determination of carbon Isotope
                              composition in unpurified samples: methamphetamine example, Biomed. Environ. Mass Spectrom.,
                              13, 531, 1986. © 1986 John Wiley & Sons Limited. Reproduced with permission.
                             mode measuring the intensity ratio of the m/z 59 and the m/z 58 ions of the
                                    +
                             [C H N] fragment. Synthesized products are introduced into the mass spec-
                               3  8
                             trometer through the gas chromatograph inlet without prior clean-up. The
                             measured ratios are in excellent agreement with the calculated ones as shown
                             in Table 4.5.
                                                          13
                                The artificial enrichment of  C in the compound of interest allows the
                             isotope  ratio measurements  to be made  with a “direct”  approach using a
                             conventional mass spectrometer. Data shown in  Table 4.5 indicate that a
                             variation step of 0.25% in the  C enrichment of methylamine is sufficient
                                                        13
                             for product differentiation.  Calculation indicates that this variation step
                             could be reduced by at least 50-fold with the use of an isotope ratio mass
                             spectrometer. With the development of on-line gas chromatograph/combus-
                             tion/isotope ratio mass spectrometer systems, the approach presented here
                             may well provide a sensible mechanism for monitoring controlled substances.
                             It should be further noted that the isotope approach exemplified here allows
                             sample differentiations after human consumption. Analysis of appropriate
                             metabolites may provide valuable sample source information. While scientific
                             merits and economical feasibility are considered in this study, obvious socio-
                             logical and legislative concerns remain to be addressed.


                             References

                                1.  Bricout, J., Isotope ratios in environmental studies, Int. J. Mass Spectrom. Ion
                                   Phys., 46, 195, 1982.


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