Counterfeit Adderall Containing Aceclofenac from Internet Pharmacies

A nontargeted approach based on liquid chromatography equipped with a quadrupole time-of-flight mass detector (LC-MS Q-TOF) joined to nuclear magnetic resonance (NMR) analysis allowed rapid identification and quantification of the anti-inflammatory drug aceclofenac in illegal Adderall tablets. The largest chromatographic peak had m/z = 354.030 and m/z = 376.012 matching, respectively, the ionic structures (M + H)(+) and (M + Na)(+) of a molecule M. The accurate mass data generated the molecular formula C16H13Cl2NO4. A screening of the pharmaceutical active substances having that molecular formula together with the MS/MS fragmentation pattern suggested aceclofenac. Aceclofenac structure was unambiguously confirmed by H-1 and C-13 NMR experiments. The aceclofenac content was 90 mg/tablet (RSD 2%) as detected by quantitative NMR. Information on the identity and content of illegal drugs is required for legal purposes; it supports in evaluating the effective impact on users safety, and it is useful for control laboratories using a targeted approach in their analytical activities.