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Introduction. A wastewater-based epidemiology approach was performed to estimate the drug consumption in Palermo city, the fifth largest city of Italy with a population of 671 696 inhabitants, and to investigate the monthly variability of drug loads in wastewater from different areas of the city. A seven-months detection campaign was conducted at the two wastewater treatment plants of the city. Methods. Following a pre-treatment, 32 samples of wastewater were analyzed by liquid chromatography-tandem mass spectrometry. Results. We estimated a mean cocaine use in Palermo of 0.19 g/day/1000 people, corresponding to 1.90 doses/1000 people and cannabinoids use of 2.85 g/day/1000 people, corresponding to 35.62 doses/1000 people. Amphetamines residues in wastewater were always recovered in concentrations lower than the limit of quantification. Conclusion. Our findings showed that drugs consumption in Palermo is in line with those of other Italian cities and that no significant differences on prevalence on cocaine and cannabinoids consumption were recorded in the different months of the survey, except for the summer period in a wastewater treatment plant of the city.

Electrospray Ionization and collision induced dissociation tandem mass spectrometry are usually employed to obtain compound identification through a mass spectra match. Different algorithms have been developed for this purpose (for example the nist match algorithm). These approaches compare the tandem mass spectra of the unknown analyte with the tandem mass spectra spectra of known compounds inserted in a database. The compounds are usually identified on the basis of spectral match value associated with a probability of recognition. However, this approach is not usually applied to multiple reaction monitoring transition spectra achieved by means of triple quadrupole apparatus, mainly due to the lack of a transition spectra database. The Surface Activated Chemical Ionization-Electrospray-NIST Bayesian model database search (SANIST) platform has been recently developed for new potential metabolite biomarker discovery, to confirm their identity and to use them for clinical and diagnostic applications. Here, we present an improved version of the SANIST platform that extends its application to forensic, pharmaceutical, and food analysis studies, where the compound identification rules are strict. The European Union (EU) has set directives for compound identification (EU directive 2002/657/EC). We have applied the SANIST method to identification of 11-nor-9-carboxytetrahydro-cannabinol in urine samples (an example of a forensic application), circulating levels of the immunosuppressive drug tacrolimus in blood (an example of a pharmaceutical application) and glyphosate in fruit juice (an example of a food analysis application) that meet the EU directive requirements. Copyright © 2016 John Wiley & Sons, Ltd.

The products of cannabis are the most frequently used illicit drugs of abuse detected in workplace drug-testing programs or in cases of driving under the influence of drugs. For this reason, there is a great need for sensitive and specific methods which can confirm the chronic exposure and which take account of the cut-off values that have been proposed in Italy by the GTFI Guidelines (Group of Italian Forensic Toxicologists). The method currently more appropriate for quantification of Δ9-Tetrahydrocannabinol (THC) and its major metabolite 11-nor-9-Carboxy-Δ9-THC (THCA) appears to be one that involves HPLC-MS/MS and keratin matrix. The purpose of this work, performed at the Mass Spectrometry Laboratory for Clinical Risk and Quality Control (CQRC) in A.O.U.P. “Paolo Giaccone” of Palermo, is the developing of an accurate method equally or more sensitive than those used routinely in forensic toxicology laboratories. A pre-analytical phase has seen the preparation of hair samples, comprising basic hydrolysis, and a subsequent Liquid-Liquid Extraction (LLE). In the analytical phase, the step of detection was performed using the Thermo Scientific™ Transcend™ II system which combines the online sample preparation technology TurboFlow™ with the chromatographic separation technique of High Performance Liquid Chromatography (HPLC) and the detection technique of tandem Mass Spectrometry (MS/MS) using a high sensitive Thermo Scientific™ TSQ Quantiva™ Triple Quadrupole Mass Spectrometer. During the phase of the developing method a series of experimental tests regarding the analytical conditions have been performed, on six different chromatographic columns. This has highlighted the main advantages of TurboFlow™, the adequate selectivity in the sample cleaning and the possibility of injecting more volumes of sample than the normal LC-MS techniques, leading to an appreciable increase in the sensitivity. According to the aim of the work, the latter steps of sample preparation, including LLE, were replaced with a simple hydrolyzate filtration and direct injection into TurboFlow™ system. In the light of the results we obtained it can be said that the method developed by TurboFlow™ -HPLC-MS/MS that involves the short phase of sample preparation procedure allows accurate quantification of cannabinoids in the keratin matrix. This technique, showing an adequate sensitivity, can be compared and preferred to used routine techniques. The short phase of preparation of the sample, also, results in a considerable saving of time and materials and in the reduction of possible errors caused by the operator.

INTRODUZIONE Le istituzioni europee e la comunità scientifica hanno, recentemente, definito un nuovo modello di sorveglianza attiva della potenziale diffusione delle droghe nella collettività, la Wastewater Based Epidemiology (WBE), attraverso la ricerca analitica delle molecole e dei loro metaboliti nelle acque reflue cittadine. Lo scopo di questo lavoro è stato la valutazione di una preliminare applicazione di METODIca WBE nella città di Palermo, poco studiata in precedenti analisi a livello nazionale e internazionale. METODI Sono stati prelevati 28 campioni (2 litri cad) di refluo medio delle 24 ore in ingresso ai due depuratori di Palermo (WP1=45.000 ab. eq.; WP2=330.000 ab. eq.) in un periodo compreso tra giugno e novembre 2015. I campioni sono stati prefiltrati, concentrati ed infine analizzati (200 mml) mediante tecnica di spettrometria di massa LC-MS/MS. Gli analiti ricercati sono stati Cocaina, Benzoilecgonina (BEG), THC-COOH e Amfetamine (MDA, MDE, MDMA, Metamfetamine). È stato effettuato, inoltre, il calcolo della quantità di sostanza stupefacente consumata nella popolazione (gr/die/1.000 abitanti e dosi/die/1.000 abitanti). RISULTATI I RISULTATI ottenuti sono illustrati nella tabella 1. I consumi di sostanze stupefacenti registrati nella città di Palermo (gr/die/1000 ab) sono RISULTATI i seguenti = Cocaina=0,145 (1,45 dosi/1000 ab); THC=4,37 (35,00 dosi/1000 ab), Amfetamine=Non quantificabili. CONCLUSIONI L’applicazione della metodologia WBE può essere considerata uno strumento aggiuntivo ai classici indicatori indiretti del consumo di droghe nella collettività a disposizione delle istituzioni per comprendere meglio il fenomeno delle tossicodipendenze e per attuare azioni di contrasto e politiche di educazione sanitaria più efficaci finalizzate alla prevenzione.