New psychoactive substances are defined as compounds with consciousness-changing effects and have been developed simultaneously with classical drugs. They arise through structural modifications of illegal substances and are mainly produced to circumvent laws. Availability is simple, since new psychoactive substances can be purchased from the Internet. Among them many chemical drug compound classes are chiral and thus the two resulting enantiomers can differ in their effects. The aim of this study is to develop a suitable chiral high-performance liquid chromatography separation method for a broad spectrum of new psychoactive substances using cellulose tris(3,5-dichlorophenylcarbamate) as a chiral selector. Experiments were performed by high-performance liquid chromatography in normal-phase mode under isocratic conditions using ultraviolet detection. Direct separation was carried out on a high-performance liquid chromatography column (Lux® i-Cellulose-5, 3.5 μm, Phenomenex®), available since 2016. Excellent separation results were obtained for cathinones. After further optimization, even 47 instead of 39 out of 52 cathinones showed baseline separation. For amphetamine derivatives, satisfactory results were not achieved. Further, new psychoactive substances from other compound classes such as benzofuranes, thiophenes, phenidines, phenidates, morpholines, and ketamines were partially resolved, depending on the polarity and degree of substitution. All analytes, which were mainly purchased from the Internet, were proven to be traded as racemates.
Bath salts, fumigations, cleaners and air fresheners, behind these terms substances are hidden, which count as “Legal Highs”. These fancy names are used to pretend Legal Highs as harmless compounds, to circumvent legal regulations for marketing as well as to increase the sales. Besides classic illicit drugs of synthetic origin such as amphetamines, cocaine and MDMA, the trade of these compounds, also known as new psychoactive substances (NPS), is not uncommon today. In many countries, NPS are still not subject to drug control. Among them, there are stimulants such as new amphetamine derivatives or cathinones, which possess a chiral centre. Little is known about the fact that the two possible enantiomers may differ in their pharmacological effect. The aim of this study was to test a novel HPLC column for the enantioseparation of a set of 112 NPS coming from different chemical groups and collected by internet purchases during the years 2010–2018. The CSP, namely Lux® 5 μm i‐Amylose‐1, LC Column 250 x 4.6 mm, was run in normal phase mode under isocratic conditions, UV detection was performed at 245 nm and 230 nm, injection volume was 10 μl and flow rate was 1 ml/min. With a mobile phase consisting of n‐hexane/isopropanol/diethylamine (90:10:0.1), herein, 79 NPS were resolved into their enantiomers successfully, for 37 of them baseline resolution was achieved. After increase of lipophily of the mobile phase to 99:1:0.1, another 27 compounds were baseline separated. It was found that all separated NPS are traded as racemic compounds.
Cannabis sativa is known to be the most abused illegal drug worldwide. To date it is not only used as a medicine but has been established as a lifestyle product. The most relevant phytocannabinoids represent the ingredients delta-9-tetrahydrocannabinol (9-THC) and cannabidiol (CBD), whereby only 9-THC shows a psychoactive effect. Since 2017, the so-called CBD-hemp containing CBD as main ingredient is distributed in many countries as a legal alternative. In these products, 9-THC must not exceed a certain percentage. It is hardly possible to differentiate between THC-hemp and CBD-hemp presenting a major challenge for authorities. Therefore, there is the need to develop fast and efficient analysis methods to distinguish between fibre-type, drug-type and intermediate-type cannabis products. The aim of this study was to compare two simple and inexpensive HPLC-UV and GC-FID methods for their ability to quantify phytocannabinoids in dried cannabis plant material. For this purpose, a set of 37 fresh and dried cannabis samples randomly chosen from seizures of Austrian police was subject to complementary quantification of 9-THC and CBD. After having taken into account decomposition of certain phytocannabinoids, the result of this quantitative study showed good correlation between HPLC-UV and GC-FID regardless of quantifying cannabis leaves or buds.
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