Phytochemical analysis on the seeds of a new Iranian Plantago ovata Forssk. population specimen.

In this paper, the phytochemical analysis of the seeds of a new Iranian Plantago ovata Forssk. population exemplar is reported. This phytochemical analysis was carried out by means of hydroalcoholic maceration, column chromatography, NMR and MS analyses and led to the isolation of sixteen compounds belonging to five different classes of natural compounds. After comparison with previous analyses, a clear difference about their whole phytochemical patterns could be observed in some terms. A possible explanation of this was generally given, too.

Fate of a Deep Eutectic Solvent upon Cosolvent Addition: Choline Chloride-Sesamol 1:3 Mixtures with Methanol.

The changes upon methanol (MeOH) addition in the structural arrangement of the highly eco-friendly deep eutectic solvent (DES) formed by choline chloride (ChCl) and sesamol in 1:3 molar ratio have been studied by means of attenuated total reflection Fourier transform infrared spectroscopy, small- and wide-angle X-ray scattering (SWAXS), and molecular dynamics simulations. The introduction of MeOH into the DES promotes the increase of the number of Cl-MeOH hydrogen bonds (HBs) through the replacement of sesamol and choline molecules from the chloride anion coordination sphere. This effect does not promote the sesamol-sesamol, choline-choline, and sesamol-choline interactions, which remain as negligible as in the pure DES. Differently, the displaced sesamol and choline molecules are solvated by MeOH, which also forms HBs with other MeOH molecules, so that the system arranges itself to keep the overall amount of HBs maximized. SWAXS measurements show that this mechanism is predominant up to MeOH/DES molar ratios of 20-24, while after this ratio value, the scattering profile is progressively diluted in the cosolvent background and decreases toward the signal of pure MeOH. The ability of MeOH to interplay with all of the DES components produces mixtures with neither segregation of the components at nanoscale lengths nor macroscopic phase separation even for high MeOH contents. These findings have important implications for application purposes since the understanding of the pseudophase aggregates formed by a DES with a dispersing cosolvent can help in addressing an efficient extraction procedure.

Application of a Low Transition Temperature Mixture for the Dispersive Liquid-Liquid Microextraction of Illicit Drugs from Urine Samples.

The use of psychoactive substances is a serious problem in today's society and reliable methods of analysis are necessary to confirm their occurrence in biological matrices. In this work, a green sample preparation technique prior to HPLC-MS analysis was successfully applied to the extraction of 14 illicit drugs from urine samples. The isolation procedure was a dispersive liquid-liquid microextraction based on the use of a low transition temperature mixture (LTTM), composed of choline chloride and sesamol in a molar ratio 1:3 as the extracting solvent. This mixture was classified as LTTM after a thorough investigation carried out by FTIR and DSC, which recorded a glass transition temperature at -71 °C. The extraction procedure was optimized and validated according to the main Food and Drug Administration (FDA) guidelines for bioanalytical methods, obtaining good figures of merit for all parameters: the estimated lower limit of quantitation (LLOQ) values were between 0.01 µg L-1 (bk-MMBDB) and 0.37 µg L-1 (PMA); recoveries, evaluated at very low spike levels (in the ng-µg L-1 range), spanned from 55% (MBDB) to 100% (bk-MMBDB and MDPV); finally, both within-run and between-run precisions were lower than 20% (LLOQ) and 15% (10xLLOQ).

Chitosan-Graphene Oxide Composite Membranes for Solid-Phase Extraction of Pesticides.

Solid-phase extraction (SPE) coupled to LC/MS/MS analysis is a valid approach for the determination of organic micropollutants (OMPs) in liquid samples. To remove the greatest number of OMPs from environmental matrices, the development of innovative sorbent materials is crucial. Recently, much attention has been paid to inorganic nanosystems such as graphite-derived materials. Graphene oxide has been employed in water-purification processes, including the removal of several micropollutants such as dyes, flame retardants, or pharmaceutical products. Polysaccharides have also been widely used as convenient media for the dispersion of sorbent materials, thanks to their unique properties such as biodegradability, biocompatibility, nontoxicity, and low cost. In this work, chitosan-graphene oxide (CS_GO) composite membranes containing different amounts of GO were prepared and used as sorbents for the SPE of pesticides. To improve their dimensional stability in aqueous medium, the CS_GO membranes were surface crosslinked with glutaraldehyde. The composite systems were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, thermogravimetric analysis, swelling degree, contact angle, and mechanical measurements. As the GO content increased, a decrease in surface homogeneity, an improvement of mechanical properties, and a reduction of thermal stability of the CS-based membranes were observed. The increased dimensional stability in water, together with the presence of high GO amounts, made the prepared composite membranes more efficacious than the ones based just on CS in isolating and preconcentrating different hydrophilic/hydrophobic pollutants.

Dispersive liquid-liquid microextraction, an effective tool for the determination of synthetic cannabinoids in oral fluid by liquid chromatography-tandem mass spectrometry.

In the present work, dispersive liquid-liquid microextraction (DLLME) was used to extract six synthetic cannabinoids (JWH-018, JWH-019, JWH-073, JWH-200, or WIN 55,225, JWH-250, and AM-694) from oral fluids. A rapid baseline separation of the analytes was achieved on a bidentate octadecyl silica hydride phase (Cogent Bidentate C18; 4.6 mm × 250 mm, 4 µm) maintained at 37 °C, by eluting in isocratic conditions (water:acetonitrile (25:75, V/V)). Detection was performed using positive electrospray ionization-tandem mass spectrometry. The parameters affecting DLLME (pH and ionic strength of the aqueous phase, type and volume of the extractant and dispersive solvent, vortex and centrifugation time) were optimized for maximizing yields. In particular, using 0.5 mL of oral fluid, acetonitrile (1 mL), was identified as the best option, both as a solvent to precipitate proteins and as a dispersing solvent in the DLLME procedure. To select an extraction solvent, a low transition temperature mixture (LTTM; composed of sesamol and chlorine chloride with a molar ratio of 1:3) and dichloromethane were compared; the latter (100 µL) was proved to be a better extractant, with recoveries ranging from 73% to 101 % by vortexing for 2 min. The method was validated according to the guidelines of Food and Drug Administration bioanalytical methods: intra-day and inter-day precisions ranged between 4 % and 18 % depending on the spike level and analyte; limits of detection spanned from 2 to 18 ng/mL; matrix-matched calibration curves were characterized by determination coefficients greater than 0.9914. Finally, the extraction procedure was compared with previous methods and with innovative techniques, presenting superior reliability, rapidity, simplicity, inexpensiveness, and efficiency.

Anatomy of a deep eutectic solvent: structural properties of choline chloride : sesamol 1 : 3 compared to reline.

The structural properties of the deep eutectic solvent (DES) formed by choline chloride (ChCl) and sesamol in 1 : 3 ratio have been investigated and compared to those of reline (ChCl : urea 1 : 2). An integrated approach combining small and wide angle X-ray scattering with molecular dynamics simulations has been employed and the simulation protocol has been validated against the experimental data. In the ChCl : sesamol DES, strong hydrogen bonds (HBs) are formed between the chloride anion and the hydroxyl groups of the choline and of sesamol molecules. Conversely, choline-choline, choline-sesamol and sesamol-sesamol interactions are negligible. A more extended interplay between the constituents is observed in reline where, besides the HBs involving the chloride anion, the eutectic formation is favored also by strong choline-urea and urea-urea interactions. The three-dimensional arrangement around the individual components shows that, in the ChCl : sesamol DES, the cholinium cations and the sesamol molecules are packed in such a way to maximize the interactions with the chlorine anion. This structural arrangement may favor the π-π interactions between the sesamol molecules and the aromatic species mediated by the chloride ions, providing an interpretation for the high separation rates previously observed for phenolic DESs towards aromatic compounds.

Phytochemical Analysis and Biological Activities of the Ethanolic Extract of Daphne sericea Vahl Flowering Aerial Parts Collected in Central Italy.

In this paper, the first phytochemical analysis of the ethanolic extract of Daphne sericea Vahl flowering aerial parts collected in Italy and its biological activities were reported. Eleven compounds were identified i.e., α-linolenic acid (1), tri-linoleoyl-sn-glycerol (2), pheophorbide a ethyl ester (3), pilloin (4), sinensetin (5), yuanhuanin (6), rutamontine (7), syringin (8), p-coumaric acid (9), p-anisic acid (10) and caffeic acid (11). To the best of our knowledge, compounds (1-4, 7-8 and 10) were isolated from D. sericea for the first time during this work, whereas sinensetin (5) represents a newly identified component of the entire Thymelaeaceae family. The extract was found to possess radical scavenging against both DPPH• and 2,2'-azino-bis(3-thylbenzothiazoline-6-sulfonic acid (ABTS•+) radicals, with at least a 40-fold higher potency against the latter. Moreover, chelating abilities against both ferrous and ferric ions have been highlighted, thus suggesting a possible indirect antioxidant power of the extract. Although the precise bioactive compounds remain to be discovered, the polyphenolic constituents, including phenolic acids, tannins and flavonoids, seem to contribute to the antioxidant power of the phytocomplex. In addition, the extract produced cytotoxic effects in MDA-MB-231 and U87-MG cancer cell lines, especially at the concentration of 625 µg/mL and after 48-72 h. Further studies are required to clarify the contribution of the identified compounds in the bioactivities of the extract and to support possible future applications.

Dispersive liquid-liquid microextraction using a low transition temperature mixture and liquid chromatography-mass spectrometry analysis of pesticides in urine samples.

Biomonitoring is a potent tool to control the health risk of people occupationally and non-occupationally exposed. The latest trend in bioanalytical chemistry is to develop quick, cheap, easy, safe and reliable green analytical procedures to analyse a large number of chemicals in easily accessible biomatrices such as urine. In this paper, a new dispersive liquid-liquid microextraction (DLLME) procedure, conceived to treat urine samples and based on the use of a low transition temperature mixture (LTTM), was developed and validated to analyse twenty pesticides commonly used in farm practises. The LTTM was composed of choline chloride and sesamol in molar ratio 1:3 (ChCl:Ses 1:3); its characterization via differential scanning calorimetry identified it as an LTTM and not as a deep eutectic solvent due to the occurrence of a glass transition at -71 °C. The prepared mixture was used as the extraction solvent in the DLLME procedure, while ethyl acetate as the dispersing solvent. The salting out effect (50 mg mL-1 of NaCl in a diluted urine sample) improved the separation phase and the analyte transfer to the extractant. Due to the high ionic strength and despite the density of ChCl:Ses 1:3 (1.25 g mL-1), the LTTM layer floated on the top of the sample solution after centrifugation. All extracts were analysed by high-performance liquid chromatography coupled to mass spectrometry. After optimization and validation of the whole method, lower limits of quantitation were in the range of 0.02 - 0.76 µg  L-1. Extraction recoveries spanned from 50 to 101 % depending on the spike level and analytes. Precision and accuracy ranges were 3-18% and 5-20%, respectively. The extraction procedure was also compared with other methods, showing to be advantageous for rapidity, simplicity, efficiency, and low cost. Finally, urine samples from ten volunteers were effectively analysed using the developed method.

Dispersive liquid-liquid microextraction,an effective tool for the determination of synthetic cannabinoids in oral fluid by liquid chromatography-tandem mass spectrometry / 药物分析学报

In the present work,dispersive liquid-liquid microextraction (DLLME) was used to extract six synthetic cannabinoids (JWH-018,JWH-019,JWH-073,JWH-200,or WIN 55,225,JWH-250,and AM-694) from oral fluids.A rapid baseline separation of the analytes was achieved on a bidentate octadecyl silica hydride phase (Cogent Bidentate C18;4.6 mm × 250 mm,4 μm) maintained at 37℃,by eluting in isocratic conditions (water:acetonitrile (25:75,V/V)).Detection was performed using positive electrospray ionization-tandem mass spectrometry.The parameters affecting DLLME (pH and ionic strength of the aqueous phase,type and volume of the extractant and dispersive solvent,vortex and centrifugation time)were optimized for maximizing yields.In particular,using 0.5 mL of oral fluid,acetonitrile (1 mL),was identified as the best option,both as a solvent to precipitate proteins and as a dispersing solvent in the DLLME procedure.To select an extraction solvent,a low transition temperature mixture (LTTM;composed of sesamol and chlorine chloride with a molar ratio of 1:3) and dichloromethane were compared;the latter (100 μL) was proved to be a better extractant,with recoveries ranging from 73％ to 101％ by vortexing for 2 min.The method was validated according to the guidelines of Food and Drug Administration bioanalytical methods:intra-day and inter-day precisions ranged between 4 ％ and 18 ％depending on the spike level and analyte;limits of detection spanned from 2 to 18 ng/mL;matrix-matched calibration curves were characterized by determination coefficients greater than 0.9914.Finally,the extraction procedure was compared with previous methods and with innovative techniques,presenting superior reliability,rapidity,simplicity,inexpensiveness,and efficiency.

Multi-residue determination of organic micro-pollutants in river sediment by stir-disc solid phase extraction based on oxidized buckypaper.

This paper describes a procedure for the isolation of 20 organic micro-pollutants among pesticides, drugs, recreational drugs, flame retardants from river sediments. After a solid-liquid extraction with a methanol:water (50:50, v/v) solution, the supernatant was diluted with water and cleaned up by stir-disc solid-phase extraction (SPE). The disc was made of buckypaper, a self-supporting entangled assembly of carbon nanotubes, which was used as a highly porous, two-sided, sorbent membrane. In the preliminary activation step, the membrane was oxidised for 2-hours with nitric acid to extend its extraction capability also to more polar compounds. All extracts were analysed by ultra-high-performance liquid chromatography-tandem mass spectrometry. A comparative investigation with commercial Strata-X Polymeric Reversed Phase SPE cartridges proved the effectiveness of the lab-made device. On the average, the analytes were recovered with yields around 69% (low spike level) and 80% (medium and high spike level), while only a couple of analytes exhibited values less than 50%. The relative standard deviation was always less than 20%. Limits of detections were in the range 0.02-9.9 ng g-1. The validated method was then applied for the analysis of sediment samples from different sites of the River Turia basin in the area of Valencia (Spain), finding tris(2-chloroisopropyl)-phosphate in all sediments at a level ranging from 6.9 to 387.9 ng g-1. Other compounds, such as pesticides and pharmaceuticals were more sporadically in these samples.

A low transition temperature mixture for the dispersive liquid-liquid microextraction of pesticides from surface waters.

This paper illustrates the development of a procedure based on the use of a low transition temperature mixture (LTTM) for the dispersive liquid-liquid microextraction (DLLME) of fungicides, insecticides and acaricides from surface waters. The LTTM preparation involves the heat-mixing of choline chloride and acetylsalicylic acid in a molar ratio 1:2 (ChCl(ASA)2). The resulting mixture appears as a clear viscous liquid at room-temperature, denser than water (1.20 ±â€¯0.01 g mL-1). For its characterization, differential scanning calorimetry (DSC) provided crucial evidence to classify it as a LTTM rather than as a deep eutectic solvent (DES) since it revealed an intense glass transition at -37 °C. Large-angle X-ray scattering (LAXS) confirmed the lack of any long-distance order. Due to the LTTM immiscibility with water, an evaluation study was carried out to test ChCl(ASA)2 as an effective alternative to the conventional chlorinated solvents for DLLME. To this end, 24 pesticides were used as model compounds, extracted from surface water samples (5 mL) and analyzed by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The definitive procedure required the optimization of some key parameters such as volume of extracting solvent, type and volume of dispersing solvent, volume of the aqueous sample, LTTM dispersion procedure, and extraction time. Depending on pKa and logP values, recoveries ranged from 18 (for very polar compounds) to 96%, revealing that the ideal candidates for the extraction with ChCl(ASA)2 are neutral compounds with logP >2. After complete validation, the method was applied to analyze water samples from the River Tiber where dodine and dimetomorph were found at low µg L-1 concentration levels.

Anti-Candida Biofilm Activity of Pterostilbene or Crude Extract from Non-Fermented Grape Pomace Entrapped in Biopolymeric Nanoparticles.

Polymeric nanoparticle-based carriers are promising agents to deliver drugs to cells. Vitis vinifera phenolic compounds are known for their antifungal activity against Candida albicans. The aim of the present study was to investigate the antifungal activity of pterostilbene or crude extracts from non-fermented grape pomace, entrapped in poly(lactic-co-glycolic) acid nanoparticles (NPs), with diameters of 50 and 150 nm, on Candida biofilm. The fluorescent probe coumarin 6 was used to study the uptake of poly(lactic-co-glycolic)acid (PLGA) NPs in planktonic cells and biofilm. The green fluorescent signal of coumarin 6 was observed in Candida biofilm after 24 and 48 hours. Both pterostilbene and crude pomace extract entrapped in NPs exerted a significantly higher anti-biofilm activity compared to their free forms. The entrapment efficiency of both pterostilbene and crude pomace extract in PLGA NPs was ~90%. At 16 µg/mL, pterostilbene loaded in PLGA NPs reduced biofilm formation of 63% and reduced mature biofilm of 50%. Moreover, at 50 µg/mL, the pomace extract loaded in NPs reduced mature biofilm of 37%. These results strongly suggest that PLGA NPs are promising nanodevices for the delivery of antifungal drugs as the crude grape pomace extract, a by-product of white wine making.

Rotating-disc micro-solid phase extraction of F2-isoprostanes from maternal and cord plasma by using oxidized buckypaper as sorbent membrane.

This paper describes the development of an original micro-solid phase extraction device and its evaluation for the isolation of F2-isoprostanes (F2-IsoPs) from cord and maternal plasma samples. The unit is very simple and consists in a rotating disc (1.8 cm diameter) of oxidized buckypaper (BP), enwrapped in a polypropylene mesh pouch. Even if the selected F2-IsoPs have logP and pKa values that make them suitable candidates for their sorption on BP, several parameters were optimized to maximize recoveries: time of adsorption and desorption; stirring speed; volume, pH and ionic strength of the sample; type, volume, and fractions of the elution solvent; oxidation grade of BP. Among all, the last one was crucial in affecting extraction yields because of the analyte interactions with polar functionalities, introduced by a preliminary oxidative acid treatment. The investigation established the optimal oxidation time and highlighted the pros and cons of the acid activation step. All extracts were analyzed by means of liquid chromatography-tandem mass spectrometry (LC-MS/MS). Validation was performed according to the main FDA guidelines for bioanalytical methods. Depending on the spike level and analyte, recoveries ranged between 30 and 120% with precision and accuracy values lower than 20%. Quantitative analysis was accomplished by matrix-matched calibration curves whose determination coefficients were higher than 0.95. Lower limit of quantitation (LLOQ) spanned the range 2.45-6.77 µg L-1. The validated method was applied to the analysis of eight pairs of mother/child plasma samples, revealing the presence of 8-iso-15-keto-PGF2α and 8-iso-PGE2 at a concentration of about 10 µg L-1 in most cord plasma samples of preterm newborns.

Phytochemical profile of Euphorbia peplus L. collected in Central Italy and NMR semi-quantitative analysis of the diterpenoid fraction.

In this work, the phytochemical profile of the ethanolic extract of Euphorbia peplus L. collected in Central Italy, was reported. This specimen had never been studied before and the analysis was accomplished by means of Column Chromatography for the separation procedure and by means of NMR Spectroscopy and Mass Spectrometry for the identification step. In particular, fourteen compounds were evidenced belonging to five different classes of natural compounds i.e. triterpenoids (pentacyclic and saponin), peculiar diterpenoids (jatrophanes and pepluanes), flavonoids (flavonols), caffeoyl-quinic acids and rare disaccharides. In addition to this, a semi-quantitative analysis on the diterpenoid fraction, by means of NMR Spectroscopy, was also performed in order to provide the real quantities of these compounds in the same fraction and in the total extract. Due to the pronounced chemo variability observed in Euphorbia spp., the availability of a reliable and quick analytical technique, such as that reported in the present study, could be a useful tool in the standardization of plant materials to be used in pharmacological studies or for ethnomedicinal purposes. The technical details for both the general phytochemical analysis and the specific quantitative one, were inserted in this paper. Moreover, the chemotaxonomic and ethnopharmacological relevance of these compounds was also discussed.

Subcritical water extraction of thyreostats from bovine muscle followed by liquid chromatography-tandem mass spectrometry.

Thyreostats can be used fraudulently to promote a rapid increase in weight of breeding animals at low cost. Their severe toxicological effects impose the development of reliable analytical methods to be used in monitoring plans. This work describes an alternative approach to isolate residues of thiouracil, methyl-thiouracil, propyl-thiouracil, phenyl-thiouracil, tapazole and mercaptobenzimidazole from bovine muscle tissue. The developed procedure is based on the following three steps: i) matrix solid-phase dispersion with C18 for the preliminary sample preparation; ii) subcritical water extraction (SWE) at 160°C and 100 bar; iii) clean-up on an Oasis HLB cartridge. The quantitative determination was performed by LC-MS/MS in dual polarity ionization by using internal standardization. The SWE-LC-MS/MS method was validated according to the identification criteria of the Commission decision 2002/657/EC. The relative recoveries ranged from 72 to 97%; within-lab reproducibility was less than 18%. The decision limit and the detection capability of all analytes were below the recommended concentration, set at 10 µg kg-1, but the validation results demonstrated that this method could only be applied for screening of thiouracil and methyl-thiouracil. Besides the analytical advantages related to the use of water as solvent extraction, the procedure allowed significant removal of lipids, whose detrimental effects on instrumentation and MS sensitivity are well-known.

Screening and Assessment of Low-Molecular-Weight Biomarkers of Milk from Cow and Water Buffalo: An Alternative Approach for the Rapid Identification of Adulterated Water Buffalo Mozzarellas.

Adulteration of Mozzarella di Bufala Campana with cow milk is a common fraud because of the high price and limited seasonal availability of water buffalo milk. To identify such adulteration, this work proposes a novel approach based on the use of species-specific, low-molecular-weight biomarkers (LMWBs). Liquid chromatography-tandem mass spectrometry screening analyses identified ß-carotene, lutein, and ß-cryptoxanthin as LMWBs of cow milk, while ergocalciferol was found only in water buffalo milk. Adulterated mozzarellas were prepared in the laboratory and analyzed for the four biomarkers. Combined quantification of ß-carotene and ergocalciferol enabled the detection of cow milk with a sensitivity threshold of 5% (w/w). The method was further tested by analyzing a certificated water buffalo mozzarella and several commercial products. This approach is alternative to conventional proteomic and genomic methods and is advantageous for routine operations as a result of its simplicity, speed, and low cost.

Oxidized Buckypaper for Stir-Disc Solid Phase Extraction: Evaluation of Several Classes of Environmental Pollutants Recovered from Surface Water Samples.

This paper describes, for the first time, the use of oxidized buckypaper (BP) as a sorbent membrane of a stir-disc solid phase extraction module. The original device, consisting of a BP disc ( d = 34 mm) enveloped in a polypropylene mesh pouch, was designed to extract organic micropollutants (OMPs) from environmental water samples in dynamic mode. High-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was used to analyze the extracts. Several classes of pesticides and pharmaceuticals were chosen as model compounds to evaluate key parameters affecting the recovery rates. To this end, the effects of adsorption time, desorption time, stirring speed, type and volume of solvent, and sample volume were thoroughly examined. After optimization, a novel and in-depth study was conducted to find a correlation between physicochemical properties of the analytes and extraction yields. Recoveries were mainly governed by a combination of log P and p Ka values. As indicated, hydrophilic compounds with log P < 1 showed poor affinity for the oxidized BP, compounds having log P > 1 exhibited recoveries ranging between 50% and 100% depending on their p Ka, while compounds with p Ka between 6 and 7.5 gave low yields irrespective of their log P. The analytical method was also validated and tested as large scale screening method of OMPs in surface waters. The analysis of real samples revealed the presence of some nonsteroidal anti-inflammatory drugs, sulfonamides, and pesticides at low ng L-1 concentration levels with relative standard deviations lower than 8%.

Recent advancements and future trends in environmental analysis: Sample preparation, liquid chromatography and mass spectrometry.

Among the thousands of chemicals having potential to enter the environment, the NORMAN network has identified at least 700 substances categorized into 20 classes in the European surface waters. Pesticides, pharmaceuticals, disinfection by-products, wood preservation and industrial chemicals are the prominent classes. Since the impact of these substances on aquatic life and human health might be dramatic, action is urgently required at multiple levels; one of them is just related to the development of more and more sensible and selective analytical methods. This review highlights the latest advancements and trends in liquid chromatography-mass spectrometry based environmental analysis. Specific sections are dedicated to novelties in sample preparation, chromatographic separation and mass spectrometry detection of emerging pollutants. The review also offers insights on last generation chromatographic and extraction materials, technological progresses and innovative methodological approaches for target and non-target analysis. As numerous papers have been published in this field, this overview covers the most representative and original works published in the 2011-2016 period.

Veterinary drugs residues: a review of the latest analytical research on sample preparation and LC-MS based methods.

The world population is increasing and there is a growing demand for food, leading to intensification of farming methods and a requirement for more coadjuvants. Potential high profits sometimes lead to fraudulent use of drugs and pesticides. Veterinary drugs in particular can pose a real risk to human health if their residues are allowed to enter the food chain. Parent drugs and their metabolites can occur in foodstuffs individually or as multicomponent mixtures with enhanced adverse effects. In order to protect consumer safety, the European Union has established lists of forbidden substances, maximum residue limits for authorised drugs and precise criteria for confirmation analyses and interpretation of the results. Due to their nature and potential danger, the 'best available technique' should always be applied. Following this principle, this review examines the procedures and techniques applied to monitoring pharmaceutical products of major concern (e.g. anthelmintics, NSAIDs, corticosteroids, coccidiostats) in foods of animal origin, discussing advances over the past five years and future trends in the field of food safety. Our goal was both to focus attention on this important topic and to provide a selection of the most relevant recent papers on drug residues in foodstuffs.