PurposePhenethylamines constitute the majority of drug-related arrests in Japan. Recently, the smuggling of tert-butoxycarbonyl (t-Boc)-protected phenethylamines has become of increasing concern, because of the difficult identification of these masked substances.MethodsIn this study, a rapid and accurate method for the detection of t-Boc-methamphetamine (t-Boc-MP) by direct analysis in real time–time-of-flight-mass spectrometry (DART–TOF-MS) was developed. The efficiency of the method was evaluated by comparison with conventional gas chromatography–MS (GC–MS) and liquid chromatography–TOF-MS (LC–TOF-MS) techniques.ResultsDuring GC–MS analysis of t-Boc-MP, MP was generated in the injection port, which can lead to an analytical error. In the LC–TOF-MS spectrum, fragment ions were detected, which were generated by McLafferty rearrangement in the ion source. On the other hand, in the DART–TOF-MS analysis of t-Boc-MP, pyrolysis could be suppressed by using a micro-syringe injection method, and the fragment ions generated by McLafferty rearrangement were still observed. Moreover, protonated t-Boc-MP could be detected.ConclusionsHence, DART–TOF-MS provides a rapid and accurate method for the detection of t-Boc-MP, allowing suppression of the pyrolysis reaction and identification of both fragment ions and protonated t-Boc-MP. To our knowledge, this is the first report for detecting t-Boc-MP by MS techniques.
We have developed a quantitative method that uses GC FID and QuEChERS to measure D 9 tetrahydrocannabinol (D 9 THC) in cannabis-infused foods. Reported methods for the analysis of cannabis-infused foods typically use liquid chromatography, but obtaining D 9 THC used in these methods, with the certiˆed concentration, is di‹cult in Japan. Therefore, we attempted to apply a method, obtained from the United Nations O‹ce on Drugs and Crime, that allows the quantitative analysis of D 9 THC in herbal cannabis, hashish, and liquid using cannabinol as the reference material. In this study, the QuEChERS method, which is widely used in food analysis, was adopted. The EN 15662 salt method (EN salt method) and Enhanced Matrix Removal-Lipid method (EMR Lipid method) were compared using recovery tests for D 9 THC added to four types of food samples. The EN salt method was found to be superior to the EMR Lipid method for some foods. A similar test was conducted on six diŠerent types of foods using the EN salt method. The recovery was 95.2 to 113.5. The precision was tested at two levels of D 9 THC content in three trials over three days. The intra-day precision was 9.8 and 1.4 for 0.1 mg/g and 1 mg/g D 9 THC, respectively. The inter-day precision was 16. 6 and 4.4
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