Comprehensive Protocol for the Identification and Characterization of New Psychoactive Substances in the Service of Law Enforcement Agencies.

A non-routine, comprehensive protocol for characterization of emerging new psychoactive substances (NPS) including chemical structures, impurities, as well as crystal structures, has been developed to facilitate the work of law enforcement agencies. A set of NPS has been synthesized, identified, and characterized by various analytical methods in order to be used as certified reference standards (CRMs). Seven selected compounds (5-IT, NM-2201, MT-45, AB-CHMINACA, UR-144, 5F-PB-22, and 4-CMC) were synthesized on the laboratory scale, then the process was upscaled to semi-technical. All products were analyzed by electrospray Q/TOF-MS/MS for molecular structure identification. The presence of by-products, as well as metal impurities, arising from the performed syntheses, were characterized by reversed phase liquid chromatography (RP-HPLC) with DAD and Q/TOF-MS detection and inductively-coupled plasma with quadrupole mass spectrometer (ICP-QMS), respectively. Additionally, the crystal structures of UR-144, NM-2201, 5F-PB-22, and 4-CMC have been determined by single-crystal and powder X-ray diffraction.

Fast and efficient deposition of broad range of analytes on substrates for surface enhanced Raman spectroscopy.

The majority of analytical chemistry methods requires presence of target molecules directly at a sensing surface. Diffusion of analyte from the bulk towards the sensing layer is random and might be extremely lengthy, especially in case of low concentration of molecules to be detected. Thus, even the most sensitive transducer and the most selective sensing layer are limited by the efficiency of deposition of molecules on sensing surfaces. However, rapid development of new sensing technologies is rarely accompanied by new protocols for analyte deposition. To bridge this gap, we propose a method for fast and efficient deposition of variety of molecules (e.g. proteins, dyes, drugs, biomarkers, amino acids) based on application of the alternating electric field. We show the dependence between frequency of the applied electric field, the intensity of the surface enhanced Raman spectroscopy (SERS) signal and the mobility of the studied analyte. Such correlation allows for a priori selection of parameters for any desired compound without additional optimization. Thanks to the application of the electric field, we improve SERS technique by decrease of time of deposition from 20 h to 5 min, and, at the same time, reduction of the required sample volume from 2 ml to 50 µl. Our method might be paired with number of analytical methods, as it allows for deposition of molecules on any conductive surface, or a conductive surface covered with dielectric layer.

IDENTIFICATION CHALLENGES IN EXAMINATION OF COMMERCIAL PLANT MATERIAL OF PSYCHOTRIA VIRIDIS.

Psychoria viridis (chacruna) is a hallucinogenic plant with psychoactive properties associated with the presence of N,N-dimethyltryptamine (DMT). This species is primarily known as an ingredient of the beverage Ayahuasca, but dry leaves are also smoked by recreational users. The plant is controlled in Poland and France and its proper identification poses many challenges due to the fact that genus Psychotria is relatively large and there are other species that are easily confused with chacruna. The aim of the present work was to develop an effective authentication procedure for the dried and shredded leaves of P. viridis, to be used in comparison of chemical and botanical characteristics of its commercial products. Dried leaves of P. viridis originating from Brazil, Peru and Hawaii were purchased from Internet providers. For DMT identification, thin layer chromatography (TLC) and high performance liquid chromatography (HPLC) methods have been elaborated, validated and applied. In order to clarify the existing differences among samples, chemometric methods have been used. Botanical features and the gas chromatography tandem mass spectrometry (GC-MS) chromatograms have been analyzed using hierarchical cluster analysis (HCA). Our studies revealed significant variety among plant material marketed as P. viridis. Grouping of samples based on their micromorphology features and GC-MS results did not correspond well with the presence of DMT. Based on our results an indisputable identification of dried specimens as P. viridis is very problematic. It is necessary to postulate changes in legislation regarding regulation of P. viridis and replace it with DMT as controlled substance.