Screening of new psychoactive substances (NPS)by gas-chromatography/time of flight mass spectrometry (GC/MS-TOF)and application to 63 cases of judicial seizure

A screening method for the separation and identification of more than fifty NPS is proposed. The method is based on fast gas-chromatography/time of flight mass spectrometry (FAST-GC/MS-TOF). Thanks to the shorter and narrower capillary column and to the rapid acquisition of the TOF detector a huge number of compounds are separated in a very short time of analysis (10 min). Only a few peaks were overlapped. The possibility to apply deconvolution by the software of the GC/MS-TOF instrument allowed the unequivocal identification also for the superimposed peaks. Linearity and LOD was studied and the method was applied to 63 cases of powders seized by the judicial authority at the airport of Milano Malpensa in Northern Italy in the period 2014\u20132017

Determination of polycyclic aromatic hydrocarbons in lipstick by gas-chromatography coupled to mass spectrometry: A case history

A suitable extraction protocol based on an liquid-liquid extraction with hexane/dimethyl sulfoxide and a GC/MS method were developed and validated to determine the concentration of six prohibited Polycyclic Aromatic Hydrocarbons (PAHs; benzo[a]pyrene; dibenz[a,h]anthracene; benz[a]anthracene; benzo[j]fluoranthene; benzo[k]fluoranthene; chrysene) in lipsticks commissioned by a cosmetic company to a manufacturer. The lipsticks were produced in four different colors. Analyses confirmed the presence of benz[a]anthracene and chrysene only in two colors in a concentration of 9.3\u20139.4 ng/g. The concentration of PAHs was 250 times lower than what is considered a toxic level on the basis of what reported in the litaraure and guidances for cosmetic ingredients; therefore we could assume that the risk for consumer health was negligeble

Comparison between Lc/Uv and Gc/Fid techniques in determining N,NDimethylacetamide(Dma) in diacerein

Objectives: The aim of this work was the quantitative determination of N,N-Dimethylacetamide (DMA) as crystallization solvent in samples of Diacerein. DMA is commonly used as a solvent in the chemical, agricultural and pharmaceutical industries. However, in order to ensure product quality and to protect patients from the potentially toxic properties, the substances used as active ingredients in therapeutic drugs should not contain high levels of residual solvents. Methods: LC is commonly used in the pharmaceutical industry to check DMA in pharmaceutical products, but in this work we were interested in validating and comparing LC/UV and GC/FID techniques for determining the presence of DMA in Diacerein Results: Both methods showed good linearity, precision and accuracy with comparable LOD and LOQ. Conclusion: The GC method, however, since it uses DMSO as an internal standard, has higher analytical versatility, thus allowing the qualitative and quantitative determination of DMA at lower levels than those obtained with LC

Determination of 6-Monoacetyl-Morphine (6-MAM) in Brain Samples from Heroin Fatalities

Objective: Post-mortem brain samples from 15 deceased patients whose death was heroin related, were analyzed to determine 6-monoacetyl-morphine (6-MAM) concentrations. The samples belonged to people died between 2008 and 2014. The first eight samples were also analyzed in 2012 to determine only morphine and codeine levels. Method: A GC/MS method was studied in order to enhance sensitivity, thus helping the determination of 6-MAM whose detection is in most cases difficult because of the complexity of the biological matrix. The analytical method was validated using deuterated internal standards (IS-D3, morphine-D3 and codeine-D3) and it showed adequate specificity, linearity, LOD, LOQ precision and accuracy for the determination of the analyte of interest. Results: 6-MAM was evidenced only in the more recent samples, thus pointing out its low stability. Its concentration ranged from 15.6 to 28.9 ng/g. Morphine and codeine was also determined and a comparison was carried out between the blood and the brain levels of the three analytes. Moreover a parallel was established between the concentrations of morphine and codeine found in the brain in 2012 and 2015. Conclusion: 6-MAM determination in the brain is particularly important when discriminating between morphine assumption and heroin abuse. In fact in the cases in which it is not detectable in the blood it can be present in the brain. It was noticed that the concentrations of morphine found in the brain in 2015 are higher respect to the levels of 2012; a possible explanation could be that 6-MAM originally present in the brain has hydrolyzed to morphine, thus increasing its levels

people centred production design

This case reports on a worldwide operating SME producing floor cleaning machines. The SME distinguishes itself from its competitors by providing highly customizable high-quality products. Employees are one of the "most-valuable resources" to the management. However, the initial situation reveals significant improvement opportunities related to the employee involvement and empowerment concerning workplace re-design. The proposed subject-oriented solution aims to involve shop floor workers in workplace (re-)design by providing them structural empowerment means such as social media for suggestion proposals, discussions and negotiations. Furthermore, the newly introduced features are designed to allow for context-sensitive reporting of suggestions and errors. Context-sensitive elicitation provides the basis for analysing impacts of changes (e.g. the affected location or worker) and visualizing potential improvement areas within the shop floor. The generic suggestion and error handling process can be tailored to different organizations. The S-BPM process handling has been integrated with a semantic wiki allowing for context-sensitive workplace improvement elicitation and change propagation analysis. The evaluation reports on findings in developer workshops, focus groups and user tests conducted in parallel to the design and implementation to ensure a user-centred approach (formative part), and on findings related to the outcome of the case implementations at the given SME (summative part)

Capillary gas-chromatographic determination of spermidine in hair lotion

Biogenic polyamines, such as spermidine (SPD, NH2-(CH2)(4)-NH-(CH2)(3)-NH2), are ubiquitous polycationic molecules which play a definitive role in many biological processes such as nucleic acid metabolism, protein synthesis, and cell growth. SPD is commonly used as an ingredient in hair lotions, because it seems to promote hair growth. This work describes a capillary GC method for quantitative determination of SPD in hair lotions using 1,6-diaminohexane as internal standard, a methyl silicone capillary column, and a flame ionisation detector. Aliquots of hair lotion were treated with an alkaline aqueous solution and internal standard was added. The emulsion was extracted with diethyl ether containing ethyl chloroformate. Ether extracts, evaporated to dryness and reconstituted in ethyl acetate, were analysed by capillary GC with flame ionisation detection. Validation took into account the specificity, linearity, precision, and accuracy of the analytical method: these parameters were valid for the quantitative determination of SPD in hair lotion

Capillary gas chromatographic determination of spermidine in diet integrators

Biogenic polyamines, among which is spermidine (SPD, NH2-(CH2)4-NH-(CH2)3-NH2), are ubiquitous polycationic mols. that have a definitive role in many biol. processes, such as nucleic acid metab., protein synthesis, and cell growth. SPD is present in diet integrators because it seems to favor the hair growth. This work describes a capillary gas chromatog. (CGC) method for the quant. detn. of SPD in diet integrators using cadaverine internal std. (IS), a Me siliconic capillary column and flame-ionization detector (FID). Diet tablets, contg. SPD, are pulverized; an aliquot of powder is treated with an alk. aq. soln. and added with IS. The suspension is extd. with di-Et ether contg. Et chloroformate (ECF). The ether exts., evapd. to dryness and reconstituted in Et acetate were analyzed in CGC/FID. Derivs. of polyamines with ECF were characterized in CGC/MS too. Validation has considered specificity, linearity, precision and accuracy of anal. method; this parameters are valid for the quant. detn. of SPD in diet integrator

Catha edulis Forsk.: caratterizzazione morfo-anatomica e fitochimica

Catha edulis Forsk. (Celastraceae), nome arabo Khat, \ue8 una specie originaria dell\u2019Africa sud-orientale, ove vengono sfruttate le sue propriet\ue0 stimolanti conseguenti alla masticazione delle foglie. Da sempre, infatti, la pianta \ue8 nota per il contenuto in alcaloidi psicoattivi (catina e catinone) e, ad oggi, la corretta identificazione di questa specie ha acquisito importanza anche in ambito forense. L\u2019indagine micromorfologica pi\uf9 recente risale al 1962 [1], mentre un approccio fitochimico di studio \ue8 ampiamente descritto in un recente lavoro di review [2]. Alla luce dei dati di letteratura, il presente lavoro si propone: 1. l\u2019approfondimento della conoscenza dell\u2019anatomia fogliare attraverso tecniche di microscopia ottica ed elettronica, 2. l\u2019individuazione, mediante indagine istochimica, dei siti di accumulo degli alcaloidi e 3. l\u2019identificazione dei principi psicoattivi nella entit\ue0 oggetto di studio. A tale scopo, nell\u2019estate 2017, sono state effettuate raccolte di giovani foglie da C. edulis coltivata presso l\u2019Orto Botanico G. E. Ghirardi (Toscolano Maderno, BS). Innanzitutto, i campioni sono stati sottoposti alle procedure di preparazione standard per le indagini micromorfologiche. Le analisi condotte hanno messo in evidenza la presenza di una epidermide monostratificata rivestita da una spessa cuticola. Il mesofillo fogliare \ue8 ben differenziato in palizzata (2 strati di cellule ricche di cristalli di ossalato di calcio) e spugnoso (3-4 strati di cellule). Alcune cellule di quest\u2019ultimo, in prossimit\ue0 dell\u2019epidermide inferiore, sono caratterizzate da un denso contenuto vacuolare che \ue8 risultato positivo ai test specifici per gli alcaloidi, dimostrando cos\uec che i principi psicoattivi vengono immagazzinati a livello di tali cellule. Per la successiva indagine fitochimica il materiale vegetale \ue8 stato suddiviso in due matrici: mesofillo e fusti. I campioni sono stati sottoposti ad estrazione mediante solventi a polarit\ue0 crescente (n-esano, CH2Cl2, MeOH). Gli estratti sono stati analizzati in GC/MS, dapprima in forma non derivatizzata per una comparazione qualitativa dei fitocomplessi. In seguito, gli estratti metanolici sono stati derivatizzati con TFAA per evidenziare la presenza di catina e catinone, non visibili nell\u2019estratto non derivatizzato. Per l\u2019identificazione dei composti \ue8 stato effettuato un confronto mediante due banche dati di spettri di massa, usando come parametro di identificazione un Quality Match (QM) superiore al 90%. Nell\u2019estratto derivatizzato \ue8 stata individuata catina con QM pari al 91%. Le indagini descritte sono attualmente in corso per ulteriori approfondimenti