Improved GC/MS Derivatization Technique for Analysis of Methylone, Ethylone, Butylone, Mephedrone, and Methedrone

By: Jaspreet Kaur-Nandra; (extracted from a paper by Ryan Carrell, Isil Dilek, Ning Chang, Uma Sreenivasan, Yunming Ying, Greg Kirkovits; Cerilliant), Analytix 2013, Volume 5

Cathinone-based stimulants emerged as a regulatory and social threat in the European Union, Asia, and US in late 2010. Marketed as “bath salts” at head shops and on the internet, these synthetic cathinones offer recreational highs that mimic the effects of illegal drugs such as cocaine, methamphetamine and LSD. Packaging labels list the compounds as “not for human consumption,” a tactic used to circumvent regulatory control and maintain legal status.

Drugs such as methylone, ethylone, mephedrone, butylone and other methcathinone analogues are commonplace and as they have increased in popularity, toxicologists require certified native and labelled reference materials to accurately identify and quantify the new compounds. There have been problems with use of deuterated internal standards of these drugs due to loss of label in the GC/MS fragmentation of the derivatized compound with PFPA and BSTFA such that an alternative method was required. By freeing the base with 0.1 M sodium bicarbonate and derivatising with TFAA in controlled temperature conditions, the decomposition of the α-amino ketones was prevented. It also enables butylone and ethylone to be readily distinguished and retains the deuterium label in the fragment ions.

The synthesis of both native and deuterated cathiniones was developed for assays such as this.

These standards are part of a range of ready to use solution based certified reference standards developed by Cerilliant that are packaged in a format which preserves concentration and integrity of the material. Time saving to the toxicologist, they provide a convenient, consistent and cost-effective alternative to the individual preparation of working reference standard solutions in the analytical lab.

A copy of the full paper including mass spectra was previously presented at the Society of Forensic Toxicologists (SOFT)/ The International Association of Forensic Toxicologists (TIAFT), San Francisco, CA, September 2011

Cerilliant Analytical Standards
Cat. No. Description Concentration (as free base) in MeOH Package Size
B-045 Butylone HCl 1.0 mg/mL 1 mL
B-046 Butylone-D3 HCl 100 µg/mL 1 mL
E-071 Ethylone HCl 1.0 mg/mL 1 mL
E-072 Ethylone-D5 HCl 100 µg/mL 1 mL
M-138 Mephedrone HCl 1.0 mg/mL 1 mL
M-139 Mephedrone-D3 HCl 100 µg/mL 1 mL
M-140 Methylone HCl 1.0 mg/mL 1 mL
M-141 Methylone-D3 HCl 100 µg/mL 1 mL
M-147 Methedrone HCl 1.0 mg/mL 1 mL


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