Improving ion mass ratio performance at low concentrations in methamphetamine GC-MS assay through internal standard selection

J Anal Toxicol. 1996 Nov-Dec;20(7):592-5. doi: 10.1093/jat/20.7.592.

Abstract

In federally regulated drug testing, laboratories must identify and quantitate drugs and their breakdown products by gas chromatography-mass spectrometry (GC-MS) to a concentration that is at least 60% below the cutoff concentration for reconfirmation purposes. Use of methamphetamine-d5 as an internal standard in routine testing with derivatization by HFBA was found to contribute m/z 91 and 118 ions to the same ions from the nondeuterated methamphetamine in the specimen. This resulted in poor chromatography and occasionally caused the 91/254 and 118/254 ion mass ratios to exceed the +20% acceptance limit established in the calibration process at low concentrations. The analogues methamphetamine-d8 and -d11 were evaluated for contributions to the nondeuterated methamphetamine ion fragments. Methamphetamine-d8 produced m/z 91 and 118 ions, but in less abundance than methamphetamine-d5. Methamphetamine-d11 was found to produce little or no detectable m/z 91 or 118. Replacing methamphetamine-d5 with methamphetamine-d11 eliminates this problem and allows the assay to consistently produce ion mass ratios and acceptable chromatography sufficient for identifying and quantitating methamphetamine at 60% below the 500-ng/mL cutoff concentration.

MeSH terms

  • Gas Chromatography-Mass Spectrometry / methods*
  • Gas Chromatography-Mass Spectrometry / standards
  • Methamphetamine / analysis*
  • Reference Standards*
  • Reproducibility of Results

Substances

  • Methamphetamine