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An original, innovative, high-throughput method based on attenuated total reflectance - Fourier’s transform infrared (ATR-FTIR) spectroscopy has been developed for the proof-of-concept discrimination of fibre-type from drug-type Cannabis sativa L. inflorescences. The cannabis sample is placed on the instrument plate and analysed without any previous sample pretreatment step. In this way, a complete analysis lasts just a few seconds, the time needed to record an ATR-FTIR spectrum. The method was calibrated and cross-validated using data provided by liquid chromatography - tandem mass spectrometry (LC–MS/MS) analysis of the different cannabis samples and carried out the statistical assays for quantitation. During cross-validation, complete agreement was obtained between ATR-FTIR and LC–MS/MS identification of the cannabis chemotype. Moreover, the method has proved to be capable of quantifying with excellent accuracy (75–103 % vs. LC–MS/MS) seven neutral and acidic cannabinoids (THC, THCA, CBD, CBDA, CBG, CBGA, CBN) in inflorescences from different sources. The extreme feasibility and speed of execution make this ATR-FTIR method highly attractive as a proof-of-concept for a possible application to quality controls during pharmaceutical product manufacturing, as well as on-the-street cannabis controls and user counselling.

Volumetric absorptive microsampling (VAMS) and dried urine spot (DUS) strategies were applied for the collection of dried microsamples for anti-doping testing of low-stability peptide hormones and growth factors prohibited by the World Anti-Doping Agency (WADA). Drying, storage and transport conditions, as well as pretreatment steps, were optimised before liquid chromatography - tandem mass spectrometry (LC–MS/MS) analysis. The analytical method has been fully validated in terms of sensitivity (limits of quantitation 0.3−10 ng/mL), precision (RSD% < 6.6 %) and extraction yields (78–91 %). Dried microsample stability studies (90 days) have been performed and compared to fluid urine stability. Significantly higher losses have been observed in fluid urine stored at −20 °C (up to 55 %) and −80 °C (up to 29 %) than in dried urine microsamples stored at room temperature (< 19 %). The final microsampling and analysis protocols allow the collection of urine microvolumes, unlikely to be tampered, stably storable and shippable with no particular precautions for possible anti-doping testing of prohibited peptides and hormones.

none 2 no The term "new psychoactive substances" refers to emerging drugs of abuse whose chemical structure and psychoactive effects are similar to other already known compounds, often providing a "legal" alternative to internationally regulated drugs and mostly available via on-line retail sites. There are several categories of new psychoactive substances, such as synthetic cannabinoids, cathinone analogues, phenethylamines, tryptamines, and the need to identify and quantify an unprecedented and growing number of new compounds represents a unique challenge for toxicological and forensic analysis. The purpose of this review is to highlight biosampling, sample preparation and analysis of the most important classes of emerging drugs of abuse in biological matrices, focusing on alternatives to classical blood and urine "in tube" approach, still representing the standard routine for bioanalysis, despite inherent flaws regarding handling, stability and process feasibility. Chromatographic techniques coupled to mass spectrometry are usually exploited to identify and quantify new psychoactive substances; due to their high sensitivity and selectivity, it is possible to determine low concentrations not only in plasma and urine, but also in alternative matrices like dried blood spots, oral fluid, hair, other body fluids and tissues. Current literature on analytical methodologies applied to these samples is still limited and a more thorough validation is often required, including a comparison among the results obtained from conventional approaches and from innovative strategies, in order to determine their actual suitability. mixed Mercolini, Laura; Protti, Michele Mercolini, Laura; Protti, Michele

Patients suffering from major depression and related pathologies (feeding and eating disorders, obsessive-compulsive disorder, post-traumatic stress disorder, anxiety disorders, etc.) are usually treated with antidepressant agents belonging to several pharmacological and chemical classes; the most recent of these agents are collectively known as “new-generation antidepressants”. In these patients, therapeutic drug monitoring (TDM) with the determination of drug and metabolite blood levels is one of the most useful procedures to optimise and personalise the treatment, enhancing both effectiveness and safety. A new approach is proposed in this study, based on microsampling of both blood and oral fluid by means of volumetric absorptive microsampling (VAMS). This approach makes sampling and storage much simpler and even self- and at-home-sampling possible, while retaining reliability, vastly increasing analyte stability and reducing overall expenses. The microsamples were pretreated by means of microextraction by packed sorbent (MEPS) on C2 sorbent and analysed by liquid chromatography with sequential spectrophotometric and spectrofluorimetric detection (HPLC-UV-FL). Method validation results were satisfactory (extraction yield >84%, precision RSD < 8.9%, stability>85.0% after 3 months). Application to blood and oral fluid VAMS from patients treated with four possible different antidepressants (sertraline, fluoxetine, citalopram and vortioxetine) provided results always in good agreement with those obtained from the corresponding fluid matrices, including the levels of drug metabolites.

Oxycodone is a widely prescribed, full agonist opioid analgesic. As such, it is used clinically to treat different kinds of painful conditions, with a relatively high potential for doping practices in athletes. In this paper, different classic and innovative miniaturised matrices from blood and urine have been studied and compared, to evaluate their relative merits and drawbacks within therapeutic drug monitoring (TDM) and to implement new protocols for anti-doping analysis. Plasma, dried blood spots (DBS) and dried plasma spots (DPS) have been studied for TDM purposes, while urine, dried urine spots (DUS) and volumetric absorptive microsamples (VAMS) from urine for anti-doping. These sampling techniques were coupled to an original bioanalytical method based on liquid chromatography-tandem mass spectrometry (LC–MS/MS) for the evaluation and monitoring of the levels of oxycodone and its major metabolites (noroxycodone and oxymorphone) in patients under pain management and in athletes. The method was validated according to international guidelines, with good results in terms of precision, extraction yield and accuracy for all considered micromatrices. Thus, the proposed sampling, pre-treatment and analysis are attractive strategies for oxycodone determination in human blood and urine, with advanced options for application to derived micromatrices. Microsampling procedures have significant advantages over classic biological matrices like simplified sampling, storage and processing, but also in terms of precision (73% for DBS, >78% for DPS, >74% for DUS, >78% for VAMS). As regards extraction yield, traditional and miniaturised sampling approaches are comparable (>67% for DBS, >74% for DPS, >75% for DUS, >75% for VAMS). All dried matrices have very low volumes, leading to a significant advantage in terms of analysis feasibility. On the other hand, this also leads to a corresponding decrease in the overall sensitivity.

An original high-performance liquid chromatographic method coupled to microextraction by packed sorbent (MEPS) was developed for the therapeutic drug monitoring (TDM) of psychiatric patients treated with the recent atypical antipsychotic ziprasidone. The chromatographic separation was achieved on a RP C18 column, using an isocratic mobile phase and setting the wavelength at 320 nm. The analyte was extracted from human plasma by means of a fast and feasible innovative MEPS procedure, optimised on C2 sorbent and requiring only 100 μL of biological sample. A second pre-treatment procedure, based on solid phase extraction (SPE), has been also developed for comparison. The availability of different pre-treatment procedures allows the choice of the one best suiting the specific clinical, economic and scientific needs. The extraction yield values were always higher than 90% and sensitivity was also good, with a limit of quantitation (LOQ) of 1 ng/mL. The method was successfully applied to plasma samples from ten subjects undergoing therapy with ziprasidone, thus confirming its suitability for the TDM of psychiatric patients, in order to personalise their pharmacological treatments.

In the last few years, several cathinone analogues have appeared on the illicit drug market and proposed as an alternative to already known stimulants in several recreational settings. The World Anti-Doping Agency classified the synthetic cathinones in the Prohibited List as specified stimulants, banned in sport competitions. We developed and validated an LC-MS/MS method for the analysis of methylone, ethylone, butylone, mephedrone, 4-methylethcathinone and 3,4-methylenedioxypyrovalerone in dried urine, plasma and oral fluid samples. Volumetric absorptive microsampling has been employed as a miniaturised sampling technique for collecting dried biological samples. Chromatographic analysis was carried out on a C18 reversed phase column with a mobile phase composed of formic acid in a water/acetonitrile mixture, by using a triple quadrupole mass analyzer. The main parameters of the volumetric absorptive microsampling procedure were investigated and the method was fully validated with satisfactory results in terms of linearity, precision, absolute recovery, matrix effects, selectivity and stability. The method was successfully applied to real samples collected from cathinones users. The biosampling strategy via volumetric absorptive microsampling for urine, plasma and oral fluid could provide reliable information, with a future perspective of implementation for forensic cases as well as for sport drug testing.