Mahmoud M E, Moussa A M, Forsyth D A, Vouros P
Barnett Institute of Chemical Analysis, Northeastern University, Boston, MA 02115.
J Chromatogr. 1991 Jul 19;549(1-2):416-22. doi: 10.1016/s0021-9673(00)91453-5.
Ketones deuteriated alpha to the carbonyl have been observed to undergo significant isotope exchange on fused-silica capillary columns during gas chromatography-mass spectrometry. The residence time of the compounds on the column was found to influence the extent of isotope exchange. The degree of exchange was examined using a variety of columns and the isotope exchange was found to occur even with brand new columns. Conversion of the keto compounds into the methyloxime derivatives resulted in retention of the "correct" isotope content during gas chromatography-mass spectrometry.
已观察到，在气相色谱-质谱分析过程中，羰基α位氘代的酮类化合物在熔融石英毛细管柱上会发生显著的同位素交换。发现化合物在柱上的保留时间会影响同位素交换的程度。使用各种柱子检查了交换程度，结果发现即使是全新的柱子也会发生同位素交换。将酮类化合物转化为甲基肟衍生物可在气相色谱-质谱分析过程中保留“正确”的同位素含量。
