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Due to the increasing consumption of illicit drugs, those cases of subjects affected by dual diagnosis, namely simultaneously suffering from mental disorders and substance abuse problems, represent an urgent concern for physicians and psychiatrists. It is evident that substance abuse is associated with a significant risk of developing psychiatric syndromes and that an early beginning of abuse habits leads to proportionally higher hazards and illness severity. Dual diagnosis cases are particularly frequent in critical settings, like for example the jail, where the lack of personal freedom facilitates the onset and the worsening of mental disorders and abuse habits. Risperidone (4-[2-[4-(6-fluorobenzo[d]isoxazol-3-yl)-1-piperidyl]ethyl]-3-methyl-2,6-diazabicyclo[4.4.0] deca-1,3-dien-5-one) is one of the most frequently prescribed drugs worldwide for the management of schizophrenia and specifically in dual diagnosis patients. It is one of the so-called "atypical antipsychotics", mainly metabolised in the liver to 9-hydroxyrisperidone, a compound with similar activity. For this reason the most clinically meaningful chemical parameter during risperidone therapy is the "active moiety", i.e. the sum of risperidone and 9-hydroxyrisperidone blood concentrations. Active moiety determination in dual diagnosis patients is an important data to be considered, with the aim of personalising and optimising the pharmacological therapy, together with a reliable monitoring of the main classes of drugs of abuse and their metabolites (cannabinoids, cocaine, amphetamines, etc). For this purpose an advanced method, based on dried blood spots (DBS), has been implemented and coupled to LC-MS/MS. The high sensitivity and selectivity of LC-MS/MS and the high feasibility of DBS sampling represent a powerful and effective analytical strategy in dual diagnosis cases, where patients are non-compliant with psychiatric therapies and also abusers. Results seem to be satisfactory and applications are providing useful data for the monitoring of dual diagnosis patients.

The Goji Berry is the fruit of Lycium barbarum and Lycium chinense, two very closely related species in the Solanaceae family, native of southeastern Europe and Asia. Goji is one of the most powerful plants in Chinese herbal medicine. It is considered a national treasure in Tibet, where it is known as “the key to eternal youth”, thanks to its significant antioxidant properties. It is often cultivated for a variety of food and beverage applications within China, but increasingly today for export as dried berries, juice and pulp or grounds. The wide-ranging properties of the Goji Berry can be explained by its composition: it is extremely rich in carotenoids, Vitamins C, B1, B2 and other vitamins, minerals, antioxidants and amino acids. Various studies have shown that Goji fruits possess numerous beneficial properties, including, antioxidant, immuno-potentiating, antimutagenic, hypoglycaemic, hypolipemic, hypotensive, all of which contribute to the slowing down of the aging process. In order to fully understand the composition of these potentially beneficial fruits, it is very useful to develop innovative analytical methods, able to provide reliable measurements of their content in bioactive substances. The goal of this research is the quali-quantitative evaluation in Goji Berry samples of antioxidant phenolic compounds by means of a HPLC method coupled to spectrofluorimetric (F) detection. The HPLC-F method is fully validated and the preliminary results, obtained from the application to some real commercial samples of fresh Goji Berries, extracts and powders, are very interesting and useful to explore the nutraceutical power of these tibetan fruits.

Il presente lavoro si propone di contribuire allo studio dell’interazione tra beni culturali e ambiente, in particolare inquinamento atmosferico, prendendo in considerazione la Cattedrale di Santa Maria del Fiore a Firenze. A tale scopo sono stati effettuati dei campionamenti di strati di degrado sui tre tipi di materiale lapideo presenti, successivamente analizzati attraverso una serie di procedure analitiche finalizzate all’identificazione chimico-mineralogica dei componenti. Allo scopo di evidenziare una correlazione tra il cambiamento cromatico che interessa le superfici dei monumenti e gli inquinanti emessi dai processi di combustione, un ulteriore studio è stato realizzato mediante misure colorimetriche successivamente relazionate ai dati analitici ottenuti. Per valutare l’impatto che l’annerimento delle superfici architettoniche del monumento oggetto di studio svolge sulla percezione visiva ed ipotizzare quale potrebbe essere la distribuzione degli strati di degrado in futuro, sono state realizzare delle carte di degrado utilizzando una indagine fotografica ed una ricerca storica di fotografie riproducenti la facciata considerata. I risultati ottenuti consentono di ipotizzare future patine di degrado meno diffuse, di colore tendente al giallo-bruno, dovuto alla crescita della componente organica del particolato.

Set up of a simple, fast and cheap liquid chromatographic method to separate four macrolides and to quantify their concentrations. It was optimised evaluating mobile phase composition, column temperature and pH to provide the best resolution of these analytes. Preliminary assays are promising and the method is under validation for application to real food samples.

Important components of the palm fruit such as oils, fatty acids, semi-solid fats, vitamin E, tocopherols, carotenoids, phytosterols and flavonoids, are here identified and quantified for their importance in the nutraceutical and food industry.

Aim of this work is to develop an innovative, feasible but reliable qualitative and quantitative analysis of Ketamine and its active metabolite Norketamine in saliva samples, optimizing fast and effective pretreatment procedures and using HPLC coupled to different detection means such as spectrofluorimetry (F) and tandem mass spectrometry (MS/MS). Separation is achieved by means of RP C18 stationary phase and a mobile phase consisting in a mixture of acetonitrile and acidic aqueous buffer. The pretreatment of saliva samples is obtained by a miniaturized system of Micro Extraction by Packed Sorbent (MEPS). The preliminary results are promising and assays are in progress in order to fully validate the method.

Il presente lavoro si propone di contribuire allo studio dell’interazione tra beni culturali e ambiente, in particolare inquinamento atmosferico, prendendo in considerazione la Cattedrale di Santa Maria del Fiore a Firenze. A tale scopo sono stati effettuati dei campionamenti di strati di degrado sui tre tipi di materiale lapideo presenti, successivamente analizzati attraverso una serie di procedure analitiche finalizzate all’identificazione chimico-mineralogica dei componenti. Allo scopo di evidenziare una correlazione tra il cambiamento cromatico che interessa le superfici dei monumenti e gli inquinanti emessi dai processi di combustione, un ulteriore studio è stato realizzato mediante misure colorimetriche successivamente relazionate ai dati analitici ottenuti. Per valutare l’impatto che l’annerimento delle superfici architettoniche del monumento oggetto di studio svolge sulla percezione visiva ed ipotizzare quale potrebbe essere la distribuzione degli strati di degrado in futuro, sono state realizzare delle carte di degrado utilizzando una indagine fotografica ed una ricerca storica di fotografie riproducenti la facciata considerata. I risultati ottenuti consentono di ipotizzare future patine di degrado meno diffuse, di colore tendente al giallo-bruno, dovuto alla crescita della componente organica del particolato.

The EC TeACH project (Technologies and tools to prioritize assessment and diagnosis of air pollution impact on immovable and movable cultural heritage) sets out to understand the different types of damage on cultural heritage in different sites: Oslo (Norway), Florence (Italy), Salè (Marocco), Cologne (Germany). There was performed the characterization of damage layer including the ion compounds performed by ion chromatography (IC) and elemental composition, carried out by coupled plasma-optical emission spectrometer (ICP-OES). To understand the origin of the ions and elements detected in the black crust specimens, the data obtained during analysis were analyzed statistically using the R Project for Statistical Computing. The results achieved shows that in all cases the SO2 has been proved to have among the pollutants the priority role in damage layer formation. Moreover, there has been reflected the impact of local pollutant sources on damage processes occurring, e.g. coal combustion and emission from railway transport in case of Cologne Cathedral, the marine aerosol in case of coastal sites Sale and Oslo.

The present work focuses on the diagnosis of the damage induced by air multi-pollutants on the Centennial Hall, situated in one of the most industrialized and polluted regions of Poland, in close neighborhood of coal power stations. In order to investigate the impact of multi-pollutants on the cement built heritage samples of damage layer and underlying material were collected from the building, taking into account rain exposure (sheltered, partly sheltered and washed out areas) and analysed by range of analytical techniques: optical and scanning electron microscopy, X ray diffractometry, differential and gravimetric thermal analysis, ion chromatography, flash combustion/gas chromatographic analysis, inductively coupled plasma-optical emission spectrometer. The results obtained show that the surface deterioration of the Centennial Hall is mainly caused by deposition of SO2 and fly ash from coal combustion, and subsequent interaction with the cement components. These results for the first time demonstrate the impact of coal power stations on black crust formation on cementitious materials.

Vengono sviluppati alcuni metodi HPLC e CE per l'analisi dei principali isoflavoni della soia, metodi analitici che consentono la loro identificazione e il loro dosaggio con risultati accurati e precisi.

Nell’ambito di un progetto finalizzato allo studio delle diverse tipologie di degrado causate dall’inquinamento atmosferico a carico del patrimonio culturale costruito, in questo lavoro sono state prelevate croste nere in 4 differenti siti (3 europei e 1 nord africano) e caratterizzate mediante cromatografia ionica e spettroscopia a emissione atomica e di massa. I risultati ottenuti mostrano come in tutti i luoghi oggetto di studio, l’SO2 abbia un ruolo prioritario nella formazione delle croste nere. É stato inoltre identificato l’impatto di fonti inquinanti locali antropiche e di sorgenti naturali sul degrado degli edifici considerati, come le emissioni da combustione di carbone e da trasporto, sia ferroviario che veicolare, nel sito di Colonia, l’aerosol marino nei siti costieri di Salè ed Oslo, i sali disgelanti ad Oslo e precedenti trattamenti di restauro nel sito di Firenze.

La ricerca condotta nell’ambito dell’impatto ambientale sul patrimonio culturale ha messo in evidenza come il degrado delle superfici architettoniche è variato e continua a variare nel tempo, principalmente in seguito al cambiamento della tipologia e concentrazione degli inquinanti atmosferici. Il progetto TeACH, finanziato dalla commissione europea, ha come obiettivo l’identificazione degli inquinanti maggiormente critici, nonché le soluzioni più idonee per investigare i mutati processi di degrado, sviluppando nuovi strumenti di monitoraggio per la protezione sostenibile del patrimonio culturale. La strumentazione utilizzata nella ricerca condotta e i dati ottenuti sono presentati e discussi.

An original HPLC-F method has been developed for the analysis of resveratrol and other antioxidants (cis-resveratrol, ferulic acid) as a first step in the study of the nutraceutical properties of grape-related products. The method takes advantages of the native fluorescence of the analytes (monitored at 386 nm, exciting at 298 nm) thus obtaining high sensitivity and selectivity. The pre-treatment consists of an innovative MEPS procedure, requiring very small amounts of sample and solvents. Under the chosen conditions, it was possible to quantify the analytes in several kinds of wine, as well as in must, in "grappa" (pomace brandy) and in the other matrices

It has been recognized that buildings undergo rapid deterioration, especially in areas with high air pollutant concentrations. This work focuses on the investigation of the impact of air multi-pollutants on Burğ al Klāb (Bastion of dogs), known as the Gate Tower, in Salè (Morocco). The diagnosis of surface damage layer was performed by range of analytical techniques including optical and scanning electron microscopy, x-ray diffraction, ion chromatography, induced coupled plasma-optical emission spectroscopy and differential and gravimetric thermal analysis. The results obtained show that sulphate is the most abundant anion followed by nitrate and chloride, while calcium has the highest concentrations among the cations. Sulphate, nitrate, chloride and calcium are in higher concentrations in the walls directly exposed to traffic road, evidencing that they are connected to emission from vehicular exhaust. The CHNSO analysis identified carbon fractions, organic (OC) and elemental (EC), showing an OC/EC ratio higher than 1 in all samples. The organic carbon fraction is in general higher in samples where the highest concentration of NO3- was also detected, thus proving the strong impact mainly of diesel vehicle exhaust fumes. A decrease of lightness (L*) and chroma (C*) was also observed passing from walls protected towards traffic to more exposed ones.

Il selenio è riconosciuto quale nutriente essenziale per l’uomo in quanto presente nella struttura dell’enzima glutatione perossidasi, che ha una funzione protettiva contro il danno ossidativo cellulare. Possiede anche altre proprietà, quali l'attività anti-cancerogena e l'azione preventiva nei confronti degli effetti tossici di alcuni metalli pesanti. Tuttavia, esiste solo un ristretto intervallo di concentrazioni (50-200 µg al giorno), in cui il selenio produce effetti positivi per la salute: al di fuori di questo intervallo, si possono avere rilevanti disturbi dovuti alla sua carenza o ad avvelenamento (selenosi). È importante quindi disporre di metodi analitici precisi ed accurati in grado di rivelarle anche piccole quantità. In questo studio, è stato effettuato il controllo di qualità di alcuni integratori contenti sodio selenito utilizzando una metodica cinetica che sfrutta la sua azione catalitica nei confronti della reazione redox tra sodio solfuro e blu di metilene. In questa procedura si misura il tempo di decolorazione del blu di metilene in funzione della concentrazione di selenito. Successivamente gli stessi integratori sono stati analizzati con una metodica CE-DAD che utilizza un tampone sodio tetraborato a pH basico come elettrolita. I risultati ottenuti in modo indipendente con le due tecniche sono in buon accordo tra di loro

The available scenarios of multi-pollutants trends in Europe indicate a shift in modern urban atmospheres from and SO2 dominated situation to a multi-pollutant situation, linked to the driven role played by traffic in determining the overall pollution in urban centres. In view of the proven overwhelming influence of mobile combustion sources in determining the future urban atmosphere, “modern’’ soiling on built heritage will be likely to contain primarily organic carbon (OC). This will imply a change in composition of damage layers, which will presumably assume a yellow-brown colouration. The EC TeACH project (Technologies and tools to prioritize assessment and diagnosis of air pollution impact on immovable and movable cultural heritage) sets out to understand the different types of damage on cultural heritage that can be expected in the future, due to changes in pollutants, both in terms of typology and concentration. Results achieved within this still running project on the composition of damage layers, collected and analysed from different monuments in Europe, will be presented and discussed. Elaboration of carbon fractions data will be liked in particular to colourimetric parameters (L*, a*, b*), with the aim of exploring the application of monitoring of colour change of architectural surfaces as potential strategy for preventive conservation.

Penicillamine (DL-2-amino-3-mercapto-3-methyl-butanoic acid) is a chelating agent derived from the hydrolysis of penicillin, lacking any antibiotic properties. The therapeutic form is D-penicillamine, while L-penicillamine is toxic. This drug is used in the treatment of severe active rheumatoid arthritis and acts by reducing the number of T-lymphocytes, inhibiting macrophage function and preventing collagen from cross-linking. It is also used as a chelating agent in Wilson's disease (a rare genetic disorder of copper metabolism), in cystinuria and in the treatment of heavy metal poisoning. Adverse effects are frequent and may include: membranous glomerulonephritis, antibody-mediated myasthenic syndrome, drug-induced systemic lupus erythematosus, toxic myopathies and elastosis perforans serpiginosa. This last one may persist even after the therapy withdrawal. Thus, to evaluate toxic effects in clinical cases we are developing a method based on capillary electrophoresis coupled to laser induced fluorescence detection (CE-LIF) in specific biological matrices such as epithelium. The analysis is carried out in a fused silica capillary, using a carbonate buffer as the background electrolyte. Satisfactory sensitivity was obtained by exciting the molecule at 488 nm after a derivatisation step with 5-(iodoacetamido)fluorescein (IAF). Preliminary results are promising and the validation of the method is in progress. At the same time, we are developing another technique based on reversed phase liquid chromatography with amperometric detection to analyse penicillamine in epithelium samples

Obiettivo del lavoro è la valutazione dell'impatto dei multiinquinanti atmosferici su un edificio in calcestruzzo situato nel centro urbano di Wroclaw in Poloniia. I risultati analitici ottenuti dalla applicazione di FEG-ESEM-EDS e ICP-OES su campioni di crosta nera e materiale inalterato prelevati sulla facciata di un edificio di importanza storica-artistica sono discussi.

The work focuses on the diagnosis of the damage induced by air multi-pollutants on the Centennial Hall, situated in one of the most industrialized and polluted regions of Poland, in close neighborhood of coal power stations. In order to investigate the impact of multi-pollutants on the cement built heritage samples of damage layer and underlying material were collected from the building, taking into account rain exposure (sheltered, partly sheltered and washed out areas) and analysed by range of analytical techniques: optical and scanning electron microscopy, X ray diffractometry, differential and gravimetric thermal analysis, ion chromatography, flash combustion/gas chromatographic analysis, inductively coupled plasma-optical emission spectrometer. The results obtained show that the surface deterioration of the Centennial Hall is mainly caused by deposition of SO2 and fly ash from coal combustion, and subsequent interaction with the cement components. These results for the first time demonstrate the impact of coal power stations on black crust formation on cementitious materials.

Development of a HPLC with colulometric detection methodology to measure olanzapine (OLA) and 4-N-desmethylolanzapine (DMO) levels in specific areas of rat brain after a single dose of OLA. Preliminary results are satisfactory in terms of sensitivity and selectivity.

Two original methods were developed and compared for TDM of topiramate: one based on HPLC with fluorescence detection and one based on CE with indirect UV detectio. Both analytical methods, fully validated, have shown to be suitable for the monitoring of patients undergoing therapy with topiramate.

Messa a punto di una metodologia analitica HPLC accoppiata ad un detector elettrochimio di tipo coulombometrico settato in ossidazione per la determinazione simultanea di due farmaci (olanzapina e aripiprazolo) utilizzati nella terapia psichiatrica della schizofrenia e del disturbo bipolare.

Very few scientific studies have been dedicated to the impact of multipollutants on 20th-century built heritage. The effect of the impact of gaseous pollutants and aerosols on cement mortars in urban areas, especially the formation of black crusts, is still not well documented, making this issue a challenging area of research. The present work focuses on the evaluation of the impact of air multipollutants on the Casa Galleria Vichi, a modern concrete building dated 1911, located in the center of Florence (Italy). In order to investigate the surface damage induced by air multipollutants, samples of deterioration layers (crusts) and underlying material were collected and analysed. The results obtained from the experimental activity performed on the damage layers indicate that gypsum, due to the deposition of sulphur atmospheric compounds, is the main damage product. Furthermore the particulate matter found embedded in the gypsum matrix, shows that oil fossil fuel combustion is the main cause of building surface blackening.

E' stato messo a punto un nuovo metodo HPLC a rivelazione elettrochimica con detector coulombometrico settato in riduzione per l'analisi di clozapina e dei suoi metaboliti in plasma umano. per la procedura di clean up è stata utilizzata una nuova tecnica di microestrazione in fase solida (MEPS) che richiede un ridotto volume di campione. In attesa di convalida, la metodologia analitica utilizzata, caratterizzata da elevata velocità di esecuzione, ha fornito risultati soddisfacenti in termini di resa di estrazione e purificazione della matrice biologica.

Duloxetine ((γS)-N-methyl-γ-(1-naphthalenyloxy)-2-thiophenepropanamine, DLX) is the most recent antidepressants introduced onto the Italian market. Like venlafaxine and milnacipran, it acts as a dual serotonin and norepinephrine reuptake inhibitor (SNRI), with approximately equal potency at both transporters; DLX seems to be very efficient and to have a fast onset of action. DLX (Cymbalta®, Xeristar®, Yentreve®, Ariclaim®) is administered as enteric-coated pellets in capsules containing 20, 30 or 60 mg of active principle. The most usual dose for the treatment of depression is 60 mg/day, with a maximum suggested dose of 120 mg/day. The most common side effects are nausea, dry mouth, fatigue, insomnia, sedation, dizziness, constipation, increased sweating, increased blood pressure, decreased appetite and body weight. Furthermore, DLX overdose can present worrisome effects, such as signs of altered mental status, cardiovascular alterations with hypotension, sinus bradycardia and prolonged QTc interval. It is evident that there is a need for having on hand new, reliable analytical methods for the determination of DLX plasma levels in depressed patients. An original HPLC method coupled to solid-phase extraction (SPE) for the determination of DLX plasma levels has been developed. It is based on the use of a Genesis C8 column (150×4.6 mm I.D., 5 μm) as the stationary phase and a mixture of acetonitrile and a pH 3.0 phosphate buffer containing triethylamine (40/60, v/v) as the mobile phase. UV detection is carried out at 230 nm. Using loxapine as the Internal Standard (IS), a chromatographic run lasts 5 minutes. The sample pre-treatment employs mixed mode reversed phase – cation exchange (MCX) cartridges (30 mg, 1 mL) and only 450 µL of human plasma are needed for a complete analysis. Cartridge elution is carried out with methanol, which is then dried and redissolved in 150 µL of mobile phase, thus obtaining a threefold concentration of the analytes. Extraction yields are satisfactory, always higher than 90%. Good linearity (r2 > 0.9990) has been found in the 2-200 ng/mL DLX concentration range. Precision assays are also satisfactory, with RSD% values always lower than 5%. The method seems to be suitable for the TDM of DLX in depressed patients' plasma.

On the subject of ancient hydraulic mortars, very few studies are reported in the literature regarding the origin, composition and identification of the various degradation typologies. Therefore, little is known on the effects of atmospheric pollutants, particularly those due to the dry and wet deposition of sulphur and carbon compounds, on the hydraulic mortars used in historic monuments, and few quantitative data are available. In fact, water from rising damp and sea spray are generally considered to be the only sources of sulphates, while the effects of sulphur of atmospheric origin on these materials are almost completely ignored. In an effort to fill the gap in knowledge, samples of ancient and modern mortars were collected at Italian, Spanish and Belgian modern historic and archaeological sites. The samples were analysed in order to throw light on the effects of atmospheric sulphation. The Authors present a synthesis of the characteristics of the samples analysed, together with an assessment of the damage encountered on sample surfaces as a result of the reaction between the mortars and atmospheric pollutants.

Per una nazione come l’Italia, che possiede gran parte delle opere d’arte mondiali, la conservazione e la salvaguardia dei beni culturali costituisce un obiettivo di primaria importanza. In quest’ottica si colloca lo studio dell’impatto ambientale sul Battistero di Firenze, situato nel centro urbano della città, realizzato attraverso il campionamento dell’aerosol atmosferico presso due delle tre porte dell’edificio, ovvero Porta Nord, esposta direttamente al traffico veicolare, e Porta Sud, influenzata indirettamente dalle emissioni veicolari. Allo scopo di confrontare la composizione del particolato atmosferico in prossimità delle due porte con quella della zona circostante, un terzo campionamento è stato effettuato sul tetto del Museo dell’Opera del Duomo, sito considerato come background dell’area. Del particolato totale sospeso sono stati misurati la concentrazione in massa in atmosfera, la componente ionica solubile e il carbonio non carbonatico. I risultati ottenuti indicano nei processi di combustione le principali sorgenti di particolato atmosferico nel centro di Firenze. Presso la Porta Nord del Battistero, le emissioni da traffico veicolare contribuiscono in modo rilevante alle concentrazioni degli inquinanti misurati. Inoltre, lo studio dimostra che, anche all’aperto, il flusso di visitatori incrementa la quantità d’aerosol atmosferico, influenzandone la composizione. Ogni monumento situato all’aperto è quindi esposto agli agenti inquinanti caratteristici della zona in cui è ubicato e solo un ampio monitoraggio locale può fornire i dati necessari per individuare strategie idonee alla protezione e conservazione del patrimonio culturale.

Homovanillic acid (HVA, 4-hydroxy-3-methoxyphenylacetic acid) is one of the main metabolites of dopamine and can thus be used as an index of dopamine metabolism which is involved in reward systems, emotional responses, personality trait expression and psychopathological phenomena. The changes occurring in the levels of HVA can be of great importance for the diagnosis of behavioural disorders. Therefore, it is fundamental that reliable analytical methods are available for the determination of homovanillic acid in human plasma. A HPLC method with amperometric detection is currently under development for this purpose and preliminary results seem to be quite promising. Homovanillic acid is analysed on a C8 column (250×4.6 mm I.D., 5 µm) with a mobile phase composed of MeOH and a pH 4.8 citrate buffer (10:90) also containing octanesulfonic acid and EDTA. Electrochemical detection is carried out using an Antec Decade amperometric detector (working electrode: glassy carbon; reference electrode: Ag/AgCl; auxiliary electrode: stainless steel) set at + 0.800 V. Solid-phase extraction (SPE) on strong anion exchange (SAX) cartridges was chosen for sample purification and pre-concentration. After conditioning, 500 µL of plasma are loaded onto the cartridge, followed by suitable washing and elution, obtaining a final sample volume of 250 µL (1:2 pre-concentration). Assays are currently underway to validate the method and to apply it to plasma samples from "at risk" adolescents for studies regarding neuroendocrine responses.

Al fine di ottenere un quadro esaustivo relativo alle più importanti alterazioni superficiali, che i principali materiali (pietre e malte) utilizzati per le decorazioni parietali del loggiato inferiore dell'Archiginnasio presentano, sono stati prelevati ed analizzati, attraverso svariate metodologie analitiche, una serie di campioni scelti sulla base della importanza storico-artistica delle decorazioni parietali e dello stato di degrado riscontrato. I dati ottenuti hanno permesso di caratterizzare i materiali e di valutarne il degrado in un ambiente esposto alla deposizione di inquinanti atmosferici. Sono state inoltre identificate le componenti atmosferiche (gas e aerosol emessi da sorgenti antropiche o naturali) responsabili del processo di degrado.

In order to evidence both the products of damage reactions and the components due to atmospheric deposition, and to identify the pollutant sources, specimens of damaged stone, consisting of surface black crusts with underlying unaltered material, were sampled on the blackened façade of the Corner Palace on the Canal Grande in Venice and submitted to a combination of physico-chemical analytical techniques. The samples were observed in thin section under optical microscope, and the damaged surface was investigated using a scanning electron microscope. X-ray diffractometric analyses, gravimetric and differential thermal analyses, and ion chromatographic analyses were performed in order to identify the main crystalline species, quantify gypsum and carbonate, and measure the anion concentrations, respectively. Finally, the carbon fractions were discriminated and measured following a chemical-thermal methodology specifically developed for damage layer specimens. The data obtained indicate gypsum as the main product of damage processes occurring due to wet and dry SO2 deposition. The burning of fossil fuels produces gases, smoke and particulate carbonaceous matter that deposit on building surfaces and react with the underlying calcareous materials forming the damage layer. Carbonaceous particles have a catalytic effect on CaSO4·2H2O formation and the ensuing surface blackening on building exteriors.

Il monitoraggio del particolato atmosferico riveste fondamentale importanza nella protezione del patrimonio culturale in quanto, per garantirla, è indispensabile conoscerne la composizione, in particolare della frazione solubile. Attualmente pochi sono i dati disponibili relativi a misure effettuate in prossimità dei monumenti. Il dosaggio della componente carboniosa nel particolato atmosferico risulta poi estremamente problematica e complessa. Nel presente lavoro, che ha lo scopo di fornire indicazioni utili ai responsabili della protezione e conservazione dei beni culturali, agli urbanisti e gestori del traffico e ai legislatori responsabili delle direttive di qualità dell’aria, vengono riportati alcuni risultati preliminari relativi alle indagini analitiche effettuate sull’aerosol atmosferico presso le Porte Nord e Sud del Battistero di Firenze. Le misure effettuate interessano la componente ionica e il carbonio non carbonatico. Il campionamento è stato eseguito utilizzando filtri in policarbonato, per le analisi in cromatografia ionica, e filtri di quarzo per le analisi della componente carboniosa. Dalla elaborazione dei dati analitici ottenuti nel corso del primo anno di monitoraggio e dei parametri metereologici e microclimatici rilevati, sono emerse importanti indicazioni riguardo le sorgenti di emissione dei principali inquinanti atmosferici presenti nell’area circostante le due Porte oggetto di studio del Battistero di Firenze e correlati con il degrado del materiale lapideo del monumento.

La sertralina, (1S,4S)-4-(3,4-diclorofenil)1,2,3,4-tetraidro-1-naftil(metil)ammina, è un derivato della naftalenammina con predominante attività farmacologica inibitoria del reuptake presinaptico della serotonina. La sertralina è indicata per il trattamento della depressione maggiore, attacchi di panico, disturbi ossessivo compulsivi e stress post traumatico. Questo farmaco è somministrato per os in dosi giornaliere comprese tra 50 e 200 mg e poiché viene assorbito lentamente, un'unica somministrazione giornaliera è terapeuticamente efficace. La sertralina subisce un intenso metabolismo di primo passaggio ad opera del CYP450, è bio-trasformata in desmetil-sertralina, un metabolita debolmente attivo che si accumula in alte concentrazioni nel plasma allo "steady state". I livelli plasmatici terapeutici della sertralina sono compresi tra 2.8 e 112 ng/mL, sebbene con pronunciata variabilità interindividuale. Il farmaco non è esente da effetti collaterali, come ad esempio perdita dell’appetito, nausea, insonnia, che sono dose-correlati. Nel presente lavoro viene descritto un rapido e preciso metodo HPLC per la determinazione di sertralina e desmetil-sertralina in plasma umano. La separazione della sertralina e della desmetil sertralina è stata ottenuta utilizzando come fase stazionaria una colonna a fase inversa C8 e come fase mobile una miscela di tetrametilammonio perclorato e acetonitrile (50/50, v/v). La rivelazione spettrofotometrica degli analiti è stata effettuata a 230 nm. Un selettiva ed efficiente purificazione dei campioni plasmatici dalla matrice biologica è stata sviluppata per mezzo di una procedura estrattiva in fase solida che consente di concentrare il campione migliorando la sensibilità del metodo. La procedura analitica sviluppata è stata applicata all'analisi di sertralina in plasma di pazienti depressi in terapia farmacologica con Zoloft® 50 mg. Il metodo proposto sembra promettente per il TDM (Therapeutic Drug Monitoring) della sertralina come strumento per una giusta personalizzazione della terapia e attenta valutazione della compliance del farmaco e delle interazioni farmacologiche in pazienti in terapia con sertralina.

Homovanillic acid (HVA, 4-hydroxy-3-methoxyphenylacetic acid) is one of the main metabolites of dopamine; for this reason, the monitoring of its levels in human plasma can be a useful research tool for assessing physiological and pathological conditions. In fact, HVA concentrations in human blood can be used as markers for neuroblastoma, and may be the expression of dopamine metabolism which is involved in reward systems, emotional responses, personality traits and psychopathology. The changes occurring in the levels of HVA could be of great importance for the diagnosis of behavioural disorders, therefore, it is important to have at disposal reliable analytical methods for the determination of HVA in human plasma. A rapid and feasible HPLC method has been developed for this purpose. Chromatographic analysis is carried out on a C8 reversed-phase column, using a mobile phase composed of acetonitrile, methanol and aqueous phosphate buffer. Coulometric detection has been used to obtain the highest sensitivity, and is carried out as follows: conditioning cell set at +100 mV; analytical cell set at detector 1 = -200 mV and detector 2 = +500 mV. Under these experimental conditions HVA is detected as a neat oxidation peak with a retention time of 6.2 minutes. The application of the method to plasma samples requires a careful sample pre-treatment step, which is carried out by means of a solid-phase extraction procedure. A 500-µL aliquot of plasma is loaded onto a C8 (50 mg, 1 mL) cartridge after addition of pH 2.5 phosphate buffer; the analyte is then eluted with the mobile phase. Preliminary assays with this procedure provided satisfactory extraction yield values, as well as good sample purification from matrix interference. The method seems thus to be promising for a sensitive and selective determination of HVA in human plasma.

The work aims to improve knowledge on the role of black crusts in stone decay, their relationship with the carbonaceous particle content of the atmosphere, and surface blackening rate. Because of the diversity of urban atmospheric pollution, different target sites have been selected among European cities, in order to investigate the formation of damage layers on monuments built in low porous carbonate stone. This report lists the results of an analysis of black crusts from the Vittoriano Monument in Rome, a crucial site for the study of cultural heritage protection in the Mediterranean basin.

It is generally agreed that the role played by aerosols in determining the air quality in urban areas is steadily increasing. As well as being among the main agents responsible for today’s atmospheric pollution, atmospheric particles are also recognized to participate actively in damage layer formation. In fact, recent years have witnessed a marked acceleration in surface soiling phenomena, as can be observed in the continual blackening of monument surfaces located in polluted areas. While numerous authors have performed detailed studies on the impact of the sulphation process in monument decay on a world-wide scale, surface blackening remains in need of in-depth investigation. The EC project CARAMEL (Carbon content and origin of damage layers in European monuments) has as one of its fundamental work steps the analytical study of black crusts collected at different monuments located in European urban sites. The aim is to create a data base of the carbon fraction concentrations present, and understand their relationship with the content of aerosol carbon components.

The principal aim of the present work is to analyse the alteration products due to reactions between atmospheric components and one of the most common limestone utilised to build the Tower of London, in order to identify the pollutant sources and the damage mechanisms affecting the masonry. The samples were characterized using classical analytical methodologies associated with new methodologies specifically set up during the CARAMEL Project to obtain quantitative data on crust compositions. Gypsum is the main constituent of the damage layers, originating from the sulphation process that occurs as a result of SO2 deposition. Moreover, black crusts reveal different physical and chemical features from those of thin grey-brownish damage layers, a finding that reflects the changes in the pollution sources contributing to crust formation.

The availability of a correct, accurate and reproducible analytical method for a complete carbon balance in black crusts is of major importance in understanding the effects of the interaction between atmospheric pollutants and the environment, particularly in the partitioning of pollutant sources, damage mechanism identification, and a sustainable protection of cultural heritage. The EC Project CARAMEL has among its primary goal the setting up of a suitable and reliable analytic technique able to distinguish and measure carbon fractions in damage layers, particularly elemental carbon. The presence of a significant amount of carbonate carbon and the removal of organic carbon are critical steps in the measurement of carbon compounds in black crusts. A chemical-thermal methodology for carbon analyses in black crusts was set up, whose specificity, accuracy and precision was tested on appropriate standard samples. The results obtained indicate that the methodology satisfactorily distinguishes among carbon species and allows a reliable evaluation of their quantities in damage layers.

Le patine di ossalato di calcio rappresentano una delle forme di alterazione più conosciuta dei monumenti lapidei. In questo lavoro, alle analisi di routine sulle patine di ossalato di calcio campionate alla superficie di murature storiche dell'isola di Torcello (VE), sono state associate analisi isotopiche.