Drug Testing and Analysis

Detection assays for drugs and methods of sports doping published between 2010 and 2011 are critically reviewed and evaluated in context with the Prohibited List 2011 as established by the World Anti- Doping Agency

This paper provides characterization of buphedrone and pentedrone, two new designer drugs encountered in Canada, by FTIR, FT-Raman, NMR, GC/MS and ESI-HRMS.

Thirteen 5-methoxy-2-methyl-N,N-dialkyltryptamines were prepared and analyzed by 1H and 13C NMR, GC-EI-MS and GC-CI-MS/MS. This study represents an extension from previous work on isomeric counterparts that carried the 5-ethoxyindole nucleus. The presentation of these data aims to support the forensic and clinical scientists to carry out their work when dealing with new psychoactive substances that appear on the market.

3β-(4-Fluorobenzoyloxy)tropane (fluorotropacocaine) (1) and its 3α isomer (2) were synthesized and characterized. Their EI and ESI mass spectra were found to be quite similar and any differences would prove inadequate for satisfactory identification. However GC and LC separations were readily achieved and coupled with mass spectrometry, both techniques successfully allowed the identification of the β isomer in case samples purchased from head shops. ¹⁹F NMR spectroscopy was also found to be useful for distinguishing the isomers.

Multiple response simultaneous optimization by using the derringer's desirability function was used for the development of a capillary electrophoresis method for the simultaneous determination of rosiglitazone (RSG) and glimepiride (GLM) in plasma and formulations. Twenty experiments, taking the two resolutions, the analysis time and capillary current as the responses with three important factors, buffer morality, volte and column temperature, were used to design mathematical models. The experimental responses were fitted into a second order polynomial and the six responses simultaneously optimized to predict the optimum conditions for the effective separation of the studied compounds. The separation was carried out by using capillary zone electrophoresis (CZE) with a silica capillary column and diode array detector at 210 nm. The optimum assay conditions were: 52 mmol l⁻¹ phosphate buffer, pH 7 and voltage of 22 kV at 29°C. The method showed good agreement between the experimental data and predictive value throughout the studied parameter space. The assay limit of detection was 0.02 μgml⁻¹ and the effective working range at relative standard deviation (RSD) of ≤ 5% was 0.05– 16 μgml⁻¹ (r = 0.999) for both drugs. Analytical recoveries of the studied drugs from spiked plasma were 97.2– 101.9 ± 0.31– 3.0%. The precision of the assay was satisfactory; RSD was 1.07 and 1.14 for intra- and inter-assay precision, respectively. The proposed method has a great value in routine analysis of RSG and GLM for its therapeutic monitoring and pharmacokinetic studies.

OMP in aqueous solution is very unstable, representing a serious difficulty for its quality control. It does not show native fluorescence, but when it is exposed to UV radiation generates a degradation product highly fluorescent which has adequate stability for indirect OMP quantification. The new analytical spectrofluorimetric method proposed here has a best precision, based on the optimization of the degradation conditions.

The analysis of human insulin from vitreous humor by means of immunopurification and LC-MS(/MS) is shown to support forensic analyses in case of fatal insulin intoxication.