Rare earth elements sediment analysis tracing anthropogenic activities in the stratigraphic sequence of Alagankulam (India).

A methodological approach based on rare earth elements analysis was developed to observe human activities in the stratigraphic sequence of Alagankulam. The site was one of the main ancient ports in south-eastern India and one of the transoceanic connecting points between East and West during the Classical Period. The sampled sediments where collected from vertical profiles, areas with traces of firing activities and filled deposits.

The casts of Pompeii: Post-depositional methodological insights.

The casts of Pompeii bear witness to the people who died during the Vesuvius 79 AD eruption. However, studies on the cause of death of these victims have not been conclusive. A previous important step is the understanding of the post-depositional processes and the impact of the plaster in bones, two issues that have not been previously evaluated.

Biomonitoring of polycyclic aromatic hydrocarbons in the urine of lactating mothers: Urinary levels, association with lifestyle factors, and risk assessment.

Polycyclic aromatic hydrocarbons (PAHs) are pollutants produced during incomplete combustion of organic matter and several industrial processes. Humans can be exposed to PAHs through ingestion of food, inhalation of tobacco smoke or polluted air, and dermal contact, causing immunologic, developmental, and reproductive problems. In the present research, eleven metabolites of PAHs were analyzed in the urine of 110 lactating women living in Spain (2015).

Determination of Third-Generation Synthetic Cannabinoids in Oral Fluids.

A procedure has been developed for the determination of third-generation synthetic cannabinoids in oral fluid samples by using a semi-automated microextraction by packed sorbent (MEPS) procedure and gas chromatography-mass spectrometry (GC-MS) determination. Five synthetic cannabinoids were employed as model compounds 5F-ADB, MMB-CHMICA, THJ-2201, CUMYL-4CN-BINACA and MDMB-CHMCZCA. The most adequate operative conditions for MEPS were evaluated giving quantitative recoveries, from 89 to 124%, in synthetic and field saliva samples spiked with 125 and 250 μg/L of the studied cannabinoids, with the exception of MDMB-CHMCZCA in field saliva samples that provided slightly lower recoveries from 62 to 66%.

Risk assessment of exposure to phthalates in breastfeeding women using human biomonitoring.

In this study, we assessed the presence of 14 phthalate metabolites in the urine of 104 lactating mothers from Valencia (Spain) who took part in the human biomonitoring project BETTERMILK. Nine of the metabolites studied showed detection frequencies >80%, whereas the rest of the metabolites presented low detection frequencies (<5%). The concentrations ranged from View Article and Find Full Text PDF

Biomonitoring of non-persistent pesticides in urine from lactating mothers: Exposure and risk assessment.

The aim of the present study was to assess the exposure to pesticides in urine from Spanish lactating mothers (n = 116). Six nonspecific (dialkyl phosphates) and 20 specific metabolites of organophosphate pesticides (OPs), herbicides and pyrethroids were analyzed. The most frequently detected biomarkers were diethyl phosphate, p-nitrophenol, 3,5,6-trichloro-2-pyridinol and 3-phenoxybenzoic acid, whose geometric means were 1.

Development of a novel methodology for determination of dialkyl phosphates in human urine using liquid chromatography-tandem mass spectrometry.

In this study a fast and sensitive method was developed for the quantitative determination of six dialkyl phosphates (DAPs) in human urine using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The proposed methodology was based on liquid-liquid extraction (LLE) with diethyl ether and ethyl acetate using MgSO and NaCl, followed by liquid chromatography and mass spectrometry detection in the selected reaction mode (SRM) with negative electrospray ionization (ESI-). Detection settings were optimized by design of experiments (DoE).

Biomonitoring of parabens in human milk and estimated daily intake for breastfed infants.

In this study, we assessed the presence of four parabens in human milk of 120 mothers from Valencia (Spain) which took part in a human biomonitoring project (BETTERMILK). The detection frequency ranges of parabens were 41-60% and 61-89% for unconjugated- and total (unconjugated + conjugated)-parabens, respectively. The concentrations ranged from View Article and Find Full Text PDF

Optimization of Resolving Power, Fragmentation, and Mass Calibration in an Orbitrap Spectrometer for Analysis of 24 Pesticide Metabolites in Urine.

Mass spectrometer parameters such as Resolving Power, type of fragmentation, and mass calibration mode were optimized in the analysis of 24 pesticide metabolites in human urine using Ultra-High Pressure Liquid Chromatography coupled to Orbitrap High-Resolution Mass Spectrometer (UHPLC-HRMS). The best results were achieved with a Resolving Power of 25,000 FWHM and by applying Collision Induced Dissociation fragmentation mode (40 eV).

Spanish Results of the Second European Cardiac Resynchronization Therapy Survey (CRT-Survey II).

Introduction And Objectives: We describe the results for Spain of the Second European Cardiac Resynchronization Therapy Survey (CRT-Survey II) and compare them with those of the other participating countries.

Methods: We included patients undergoing CRT device implantation between October 2015 and December 2016 in 36 participating Spanish centers. We registered the patients' baseline characteristics, implant procedure data, and short-term follow-up information until hospital discharge.

Determination of four parabens and bisphenols A, F and S in human breast milk using QuEChERS and liquid chromatography coupled to mass spectrometry.

For the first time, a multiresidue, sensitive and high throughput method for determination of bisphenol A, F and S and 4 parabens (methyl paraben, ethyl paraben, propyl paraben and butyl paraben) in human breast milk was developed. The proposed method includes an extraction and clean-up procedure based on QuEChERS methodology followed by liquid chromatography coupled to triple quadrupole mass spectrometry determination. Negative atmospheric pressure chemical ionization in the selected reaction monitoring mode was used for mass detection.

Biomonitoring of bisphenols A, F, S in human milk and probabilistic risk assessment for breastfed infants.

The present study addresses the presence of bisphenols A (BPA) and its analogs bisphenol F (BPF) and S (BPS) in milk of 120 mothers living in Valencia (Spain) and participating in the BETTERMILK project (year 2015). We also studied the factors that could influence the BPA levels and estimated the exposure and the risk for breast fed infants. The frequency of detection of total (conjugated + unconjugated) and unconjugated-BPA were 83% and 77%, with a geometric mean of 0.

Assessment of air passive sampling uptakes for volatile organic compounds using VERAM devices.

A calibration chamber has been designed and employed for the simple and easy determination of uptake sampling rate (R) of volatile organic compounds (VOCs) from air using passive samplers. A flow of clean air was continuously spiked, at a constant VOC concentration, by the microinjection of a standard solution by means of a T-type tube. The developed system allowed the complete evaporation at room temperature of the standard solution in acetone and the air concentration of VOCs was easily controlled by the regulation of the clean air flow, the standard solution concentration and its flow.

Poisoning histories in the Italian renaissance: The case of Pico Della Mirandola and Angelo Poliziano.

Giovanni Pico della Mirandola and Angelo Poliziano were two of the most important humanists of the Italian Renaissance. They died suddenly in 1494 and their deaths have been for centuries a subject of debate. The exhumation of their remains offered the opportunity to study the cause of their death through a multidisciplinary research project.

Ultrastructural Alterations of Midgut Epithelium, But Not Greater Wing Fluctuating Asymmetry, in Paper Wasps (Polistes dominula) from Urban Environments.

Polistes paper wasps can be used to monitor trace metal contaminants, but the effects of pollution on the health of these insects are still unknown. We evaluated, in a south-eastern area of Spain, whether workers of Polistes dominula collected at urban and rural sites differ in health of midgut tissue and in fluctuating asymmetry, an estimate of developmental noise. We found that wasps collected at the urban sites had abundant lead (Pb)-containing spherites, which were less visible in wasps from the rural sites.

Hard cap espresso extraction-stir bar preconcentration of polychlorinated biphenyls in soil and sediments.

A Nespresso hard cap espresso machine has been employed for the quantitative extraction of polychlorinated biphenyls (PCBs) from sediments and soils. Sample extraction was performed from five grams of sample in less than 40 s, with 200 mL ethanol 40% (v/v) in water and PCBs were concentrated using stir bar sorptive extraction (SBSE) and determined by thermal desorption-gas chromatography-tandem mass spectrometry (TD-GC-MS-MS). Eleven PCB congeners (28, 52, 77, 80, 81, 101, 118, 138, 153,169, and 180) were determined in soils and sediments with limits of quantification in the 0.

Prediction of alkaline earth elements in bone remains by near infrared spectroscopy.

An innovative methodological approach has been developed for the prediction of the mineral element composition of bone remains. It is based on the use of Fourier Transform Near Infrared (FT-NIR) diffuse reflectance measurements. The method permits a fast, cheap and green analytical way, to understand post-mortem degradation of bones caused by the environment conditions on different skeletal parts and to select the best preserved bone samples.

Use of a versatile, easy, and rapid atmospheric monitor (VERAM) passive samplers for pesticide determination in continental waters.

The versatile, easy, and rapid atmospheric monitor (VERAM), a passive sampler device widely used for air monitoring, was evaluated as passive sampler for the determination of 23 pesticides in water. Gas chromatography with mass spectrometry detection was employed for determination of pesticides after microwave-assisted-extraction and specific clean-up of deployed samplers. The proposed methodology reached method detection levels from 2 to 10 ng pesticide per sampler.

Target analysis and retrospective screening of veterinary drugs, ergot alkaloids, plant toxins and other undesirable substances in feed using liquid chromatography-high resolution mass spectrometry.

A comprehensive strategy combining a quantitative method for 77 banned veterinary drugs, mycotoxins, ergot alkaloids and plant toxins, and a post-target screening for 425 substances including pesticides and environmental contaminants in feed were developed using a QuEChERS-based extraction and an ultra-high performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS). The quantitative method was validated after previous statistical optimisation of the main parameters governing ionisation, and presented recoveries ranging, in general, from 80 to 120%, with a precision in terms of Relative Standard Deviation (RSD) lower than 20%. The full-scan accurate mass data were acquired with a resolving power of 50000 FWHM and a mass accuracy lower than 5ppm.

Non-destructive analytical methods to study the conservation state of Apadana Hall of Persepolis.

Atmospheric and biological agents are the main enemies of the building material conservation. In this work an innovative methodological approach, based on Near Infrared Spectroscopy (NIR) and X-Ray Fluorescence Spectroscopy (XRF), has been employed to evaluate the conservation state of Persepolis limestone samples collected both, under a protective shelter and outside the shelter, at Apadana Audience Hall area in Persepolis. The use of NIR spectra permitted to discriminate, by using Principal Component Analysis (PCA), the differences between samples collected inside and outside the protective shelter and we have been able to identify a major degradation state of the out shelter stone samples due to a major presence of organic compounds.

Combined target and post-run target strategy for a comprehensive analysis of pesticides in ambient air using liquid chromatography-Orbitrap high resolution mass spectrometry.

A comprehensive strategy for the analysis of current airborne pesticides has been developed using liquid chromatography coupled to high resolution mass spectrometry. The methodology includes both quantitative target analysis and post-run target screening analysis. The quantitative method was validated after a previous statistical optimisation of the main factors governing the ion source ionization and a study of the single-stage Orbitrap fragmentation through the HCD cell.

Wide-range screening of banned veterinary drugs in urine by ultra high liquid chromatography coupled to high-resolution mass spectrometry.

In this work, an ultra high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) methodology is proposed for the multi-class multi-residue screening of banned and unauthorized veterinary drugs in bovine urine, using an Orbitrap Exactive™ analyzer working at a resolving power of 50,000 FWHM in full scan, both in positive and negative mode. The method currently covers 87 analytes belonging to different families such as steroid hormones, β-agonists, resorcylic acid lactones (RAL), stilbens, tranquillizers, nitroimidazoles, corticosteroids, NSAIDs, amphenicoles, thyreostatics and other substances such as dapsone. A database including the elemental composition, the polarity of acquisition, retention time and expected adducts was built for the targeted analysis, and a high mass accuracy (<5 ppm) was set as one of the identification criteria.