Risk factors for partial adherence to parenteral antipsychotics in outpatients with severe mental disorders

Heavy Metal Contents in Soft-Bottom Marine Macrophytes and Sediments Along the Mediterranean Coast of Spain

. Hg, Cd, Pb and Zn concentrations were determined in sediment and in tissues of five species of soft-bottom marine macrophytes (Posidonia oceanica, Cymodocea nodosa, Zostera noltii, Ruppia cirrhosa and Caulerpa prolifera) along the Spanish Mediterranean coast. Levels of metals were low in most of the sampling stations and similar to those found by other authors in uncontaminated zones. Certain locations, however, showed some degree of contamination (Cambrils, Almassora, Alacant, Mar Menor and El Portus). In Santa Pola we found high contents of metals in one sample of sediment due to the high proportion of the fine fraction (particules < 63µm) and organic matter, but not in the seagrass spe…

Determination of PAHs in airborne particles by accelerated solvent extraction and large-volume injection-gas chromatography-mass spectrometry.

Abstract A sensitive and automated method is presented for the determination of polycyclic aromatic hydrocarbons (PAHs) in airborne particulate matter. The procedure includes extraction of PM10-bound PAHs by accelerated solvent extraction (ASE) followed by gel permeation chromatography (GPC) clean-up, and large-volume programmable temperature vaporizer (PTV–LV) injection coupled to GC–MS. The limit of detection (LOD) of the whole method, based on a signal-to-noise ratio (S/N) of 3:1, ranged from 0.26 pg m−3 to 3 pg m−3 when air volumes of 760 m3 are collected. The hexane–acetone mixture (1:1, v/v) gave the best recoveries when ASE parameters were fixed at 125 °C, 1500 psi, and a total time …

Application of accelerated solvent extraction followed by gel performance chromatography and high-performance liquid chromatography for the determination of polycyclic aromatic hydrocarbons in mussel tissue.

Accelerated solvent extraction (ASE) has been evaluated as a fast alternative to methanolic saponification for the extraction of 12 polycyclic aromatic hydrocarbons (PAHs) from mussel tissue. Several solvent systems and different operating conditions were investigated. The mixture dichloromethane-acetone (1:1, v/v) gave the best recoveries at 125 degrees C and 1500 psi, in a total time of 10 min. No yield difference was found between freeze-drying (Fd) or drying the wet mussel with diatomaceous earth (Ded) prior to extraction. The ASE method was validated using the standard reference material SRM 2977, a freeze-dried mussel tissue with naturally present organic contaminants. The performance…

High performance liquid chromatography—atomic fluorescence spectrometric determination of arsenic species in beer samples

Abstract A method has been developed for the direct determination of As(III), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and As(V) in beers by hydride generation—atomic fluorescence spectrometry after separation of arsenic species by high performance liquid chromatography. Compounds were separated by anion-exchange chromatography with isocratic elution using KH 2 PO 4 /K 2 HPO 4 as mobile phase with elution times of 1.67, 2.08, 6.52 and 10.72 min for As(III), DMA, MMA and As(V), respectively. Parameters affecting the hydride generation of all arsenic species were studied and the best conditions were established as a reaction coil of 150 cm, for a sample injected volume of 100 …

Comprehensive analytical strategy for biomonitoring of pesticides in urine by liquid chromatography–orbitrap high resolution mass spectrometry

In this study we propose an analytical strategy that combines a target approach for the quantitative analysis of contemporary pesticide metabolites with a comprehensive post-target screening for the identification of biomarkers of exposure to environmental contaminants in urine using liquid chromatography coupled to high-resolution mass spectrometry (LC–HRMS). The quantitative method for the target analysis of 29 urinary metabolites of organophosphate (OP) insecticides, synthetic pyrethroids, herbicides and fungicides was validated after a previous statistical optimization of the main factors governing the ion source ionization and a fragmentation study using the high energy collision disso…

Efficiency of the microwave-assisted extraction of hydrocarbons and pesticides from sediments

Abstract A mixture of toluene and water is proposed for the microwave-assisted extraction of organic pollutants, hydrocarbons and pesticides, from marine sediments. The effect of experimental conditions, such as microwave power and irradiation time, on the extraction of linear, unresolved and polycyclic aromatic hydrocarbons as well as PCBs and DDTs has been evaluated using real marine sediment samples. Values found by Soxhlet and ultrasonic extraction were employed to evaluate the efficiency of the microwave-assisted extraction. Analytical determinations were carried out by gas chromatography using FID, ECD and MS detectors. For 2 g of a dry sediment, an extraction time of 6 min with 10 ml…

Similar subjective response and adherence rates for long-acting risperidone and conventional depots

Background and Aims:Amongst oral antipsychotics, tolerance and adherence are thought to be higher with atypicals versus conventional agents. Fewer data exist for parenteral antipsychotics regarding the atypical–conventional comparison.Aim:to compare adherence rates and subjective response between long-acting risperidone (LAR) and conventional depots.Methods:Cross-sectional, naturalistic, one-site study of all outpatients with severe mental disorders treated with injectable antipsychotics over a 12–month period at one Spanish mental health unit. Different sets of broadly– and narrowly–defined criteria for adherence were calculated from mental health nurse´s registry data. Patients´ subjectiv…

Monitoring programme on cadmium, lead and mercury in fish and seafood from Valencia, Spain: levels and estimated weekly intake.

The study was carried out to determine the current levels of mercury, cadmium, and lead in fish and seafood from the market of Comunitat Valenciana, Spain. Levels of total mercury ranged from 0.02 to 3.15 mg kg⁻¹ w.w. (average = 0.073 mg kg⁻¹ w.w.). Cadmium concentrations ranged from 0.003 to 0.66 mg kg⁻¹ w.w. (average = 0.27 mg kg⁻¹ w.w.) for seafood, and between 0.003 and 0.71 mg kg⁻¹ w.w. (average = 0.01 mg kg⁻¹ w.w.) for marine fish. Concerning lead, concentrations from 0.02 to 0.36 mg kg⁻¹ w.w (average = 0.04 mg kg⁻¹ w.w.) were found in fish, and from 0.02 to 1.02 mg kg⁻¹ w.w. in seafood (average = 0.147 mg kg⁻¹ w.w.). The levels found were, in general, lower than maximum levels propos…

Determination of organic and inorganic mercury species in water and sediment samples by HPLC on-line coupled with ICP-MS.

This paper describes a preconcentration method for Hg(2+) and MeHg(+) in water samples using sodium diethyldithiocarbamate immobilized in polyurethane foam (PU-NaDDC) and an extraction method for several mercury species in sediment samples, including MeHg(+), EtHg(+) and PhHg(+), which is simple, rapid, and uses a single organic solvent. Separation and measurement were done by high-performance liquid chromatography on-line with inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Initially, the test of recovery was applied using procedures compatible with HPLC. Under the optimum extraction conditions, recoveries of 96.7, 96.3 and 97.3% were obtained for MeHg(+), EtHg(+), and PhHg(+),…

Multivariate data analysis and bivariate regression studies applied to comparison of two multi-elemental methods for analysing wine samples

Two inductively coupled plasma mass spectrometry (ICP-MS) methods which permit multi-elemental analysis in wine samples have been compared following two strategies. First, a multivariate tool based on principal component analysis (PCA) was employed for a global (all analytes) qualitative comparison of the two methods. A single plot based on the confidence limits of the Q and T2 PCA model statistics corresponding to the ‘standard’ method results (calibration set) was used to check the comparability of the ‘candidate’ method (test samples). The residual matrix (after test matrix interpolation into the PCA model) gives qualitative information about the nature of the main errors. This approach …

Organochlorinated pesticides in sediments from the Lake Albufera of Valencia (Spain).

Bottom sediment samples from 121 sites of the Lake Albufera of Valencia were analyzed. Dieldrin, endrin, heptachlor and op'-DDT were not detected (0.01 ng g(-1)) in 88-93% of the sites. Aldrin and HCB concentration ranges were between0.01 and 0.1 ng g(-1) in 86% and 94% of the sites, respectively. Heptachlor-epoxide and lindane 95% confidence intervals were 0.2-0.5 and 0.06-0.12, respectively. The greatest average concentration corresponds to pp'-DDE, pp'-DDD and pp'-DDT. The sum of six isomers and derivatives of the DDT average concentration reaches 2.1 ng g(-1), as opposed to 2.7 ng g(-1) for the sum of 13 pesticides considered. In the site with a major contamination, 27.0 ng g(-1) of pp'…

A multinjection strategy for mercury speciation.

Abstract A multiinjection strategy has been developed to increase the sampling throughput of the high-performance liquid chromatography determination of inorganic-mercury, methylmercury, ethylmercury and phenylmercury. The method involves the injection of samples each 3.5 min, in spite of the fact that phenylmercury retention time corresponds to 9.04 min. In the selected conditions, the sampling frequency was 11 h −1 in front of that of 6 h −1 , obtained by conventional injection of each sample after the complete elution of Hg species. Additionally, the analytical reagents consumption was reduced drastically in almost 50%. The main characteristics of the chromatographic separation were main…

Passive Air Sampling

Optimization of a microwave-assisted extraction large-volume injection and gas chromatography–ion trap mass spectrometry procedure for the determination of polybrominated diphenyl ethers, polybrominated biphenyls and polychlorinated naphthalenes in sediments

Abstract A sensitive and rapid method for the determination of polybrominated diphenyl ethers (PBDEs), polybrominated biphenyls (PBBs) and polychlorinated naphthalenes (PCNs) in sediment samples is proposed. The method involving microwave-assisted extraction (MAE) and large-volume injection (LVI) gas chromatography (GC)–ion trap mass spectrometry (ITMS), and the experimental conditions were optimized using the statistical design of experiments (DOE). A Plackett–Burman (P–B) design was chosen to estimate the influence of five factors, such as resonance excitation voltage (EV), isolation time (IT), excitation time (ET), ion source temperature (IST) and electron energy (EE) on the analytical r…

Relationships between sediment physico-chemical characteristics and heavy metal bioaccumulation in Mediterranean soft-bottom macrophytes

Abstract Concentrations of Hg, Cd, Pb and Zn in the two seagrasses ( Posidonia oceanica and Cymodocea nodosa ), green alga Caulerpa prolifera and sediment and some physico-chemical characteristics of the sediment (organic matter, fine fraction (particles Significant correlations between the concentrations of metals in the plants and sediment (alone or normalized with respect to the physico-chemical characteristics) were usually found for Hg and Zn. For Pb only C . prolifera fractions were correlated to the Pb content of the sediment. For Cd no significant correlations were obtained between the metal in the plants and sediment. The concentration factors of the metals in the plants with respe…

Headspace–mass spectrometry determination of benzene, toluene and the mixture of ethylbenzene and xylene isomers in soil samples using chemometrics

A simple and fast method has been developed for the determination of benzene, toluene and the mixture of ethylbenzene and xylene isomers (BTEX) in soils. Samples were introduced in 10 mL standard glass vials of a headspace (HS) autosampler together with 150 microL of 2,6,10,14-tetramethylpentadecane, heated at 90 degrees C for 10 min and introduced in the mass spectrometer by using a transfer line heated at 250 degrees C as interface. The volatile fraction of samples was directly introduced into the source of the mass spectrometer which was scanned from m/z 75 to 110. A partial least squares (PLS) multivariate calibration approach based on a classical 3(3) calibration model was build with m…

The rapid atmospheric monitoring system of the Pierre Auger Observatory

The Pierre Auger Observatory is a facility built to detect air showers produced by cosmic rays above 1017 eV. During clear nights with a low illuminated moon fraction, the UV fluorescence light produced by air showers is recorded by optical telescopes at the Observatory. To correct the observations for variations in atmospheric conditions, atmospheric monitoring is performed at regular intervals ranging from several minutes (for cloud identification) to several hours (for aerosol conditions) to several days (for vertical profiles of temperature, pressure, and humidity). In 2009, the monitoring program was upgraded to allow for additional targeted measurements of atmospheric conditions shor…

Searching the most appropriate sample pretreatment for the elemental analysis of wines by inductively coupled plasma-based techniques.

Different sample preparation methods were evaluated for the simultaneous multielement analysis of wine samples by inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). Microwave-assisted digestion in closed vessel, thermal digestion in open reactor, and direct sample dilution were considered for the determination of Li, Be, Na, Mg, Al, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Sr, Y, Mo, Cd, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Tl, Pb, and Bi in 12 samples of red wine from Valencia and Utiel-Requena protected designation of origin. ICP-MS allows the determination of 17 elements in most…

Determination of arsenic compounds in beverages by high-performance liquid chromatography-inductively coupled plasma mass spectrometry.

Arsenic compounds including arsenous acid (As(III)), arsenic acid (As(V)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) were separated by high-performance liquid chromatography (HPLC) and detected by inductively coupled plasma mass spectrometry (ICP-MS). A Hamilton PRX-100 anionic-exchange column and a pH 8.5 K(2)HPO(4)/KH(2)PO(4) 5.0x10(-3)molL(-1) mobile phase were used to achieve arsenic speciation. The separation of arsenic species provided peaks of As(III) at 2.75min, DMA at 3.33min, MMA at 5.17min and As(V) at 12.5min. The detection limits, defined as three times the standard deviation of the lowest standard measurements, were found to be 0.2, 0.2, 0.3 and 0.5ngmL(-1) f…

Preliminary Results on the Use of Leather Chrome Shavings for Air Passive Sampling

A new passive sampler based on low-density polyethylene (LDPE) layflat tube filled with chrome shavings from tannery waste residues was evaluated to determine volatile organic compounds (VOCs) in indoor and outdoor areas. VOCs were directly determined by head space-gas chromatography-mass spectrometry (HS-GC-MS) without any pretreatment of the sampler and avoiding the use of solvents. Limit of detection values ranging from 20 to 75 ng sampler−1and good repeatability values were obtained for VOCs under study with relative standard deviation values from 2.8 to 9.6% except for carbon disulfide for which it was 22.5%. The effect of the amount of chrome shavings per sampler was studied and resul…

Microwave-assisted extraction of polybrominated diphenyl ethers and polychlorinated naphthalenes concentrated on semipermeable membrane devices

Abstract Microwave-assisted extraction (MAE) has been evaluated as an alternative to dialysis for the extraction of polybrominated diphenyl ethers (PBDEs) and polychlorinated naphthalenes (PCNs) sampled by semipermeable membrane devices (SPMDs), using gas chromatography coupled to tandem mass spectrometry (GC–MS–MS). For MAE optimization a two level full factorial design 2 3 , plus a centre point, which involves 11 randomized runs was used. The results showed that the temperature had a significant influence on the extraction of the nine PBDEs and four PCNs tested. Also, the solvent volume had a positive influence on the extraction of PBDEs and PCNs, but only in latter compounds, it achieves…

Gas chromatographic determination of organochlorine pesticides; contamination of dicofol, fenson, and tetradifon in fish and natural waters of a wet area beside the Mediterranean sea

Microwave-assisted extraction of OCPs, PCBs and PAHs concentrated by semi-permeable membrane devices (SPMDs)

Abstract Microwave-assisted extraction (MAE) has been evaluated as an alternative to dialysis for extraction of some water-borne hydrophobic contaminants sampled by semi-permeable membrane devices (SPMDs). Seven organochlorine pesticides (OCPs), 11 polychlorinated biphenyls (PCBs) and 13 polycyclic aromatic hydrocarbons (PAHs) were accumulated in SPMDs at nanogram levels and extracted with three 3-min irradiation cycles with 33 mL of a solvent mixture hexane–water (10:1,v/v) in each cycle. The developed MAE method gave for all analytes investigated statistically comparable extraction yields with those found by dialysis carried out with a total volume of 250 mL hexane for 48 h at room temper…

Determination of mercury, cadmium, chromium and lead in marine organisms by flameless atomic absorption spectrophotometry

Chemometric determination of arsenic and lead in untreated powdered red paprika by diffuse reflectance near-infrared spectroscopy.

It has been evaluated the potential of near-infrared (NIR) diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) as a way for non-destructive measurement of trace elements at microg kg(-1) level in foods, with neither physical nor chemical pre-treatment. Predictive models were developed using partial least-square (PLS) multivariate approaches based on first-order derivative spectra. A critical comparison of two spectral pre-treatments, multiplicative signal correction (MSC) and standard normal variate (SNV) was also made. The PLS models built after using SNV provided the best prediction results for the determination of arsenic and lead in powdered red paprika samples. Relativ…

Microwave-assisted extraction of pyrethroid insecticides from soil

Abstract An analytical method has been developed for the microwave-assisted extraction of synthetic pyrethroid insecticide residues in soils and their determination by gas chromatography with electron capture detector (ECD) and mass spectrometry (MS) detector. Clean soil samples were spiked with nine pyrethroids: tetramethrin, cyfluthrin, flucythrinate, deltamethrin, bifenthrin, permethrin, cypermethrin and fluvalinate were used for this study. Concentration levels were 50 ng g −1 for all the compounds studied except to sumitrin for which a 10 μg g −1 was evaluated. Two grams of sample were treated in a closed PTFE reactor with 10 mL toluene and 1 mL water and irradiated at 700 W during 9 m…

Determination of acrylamide in coffee and chocolate by pressurised fluid extraction and liquid chromatography-tandem mass spectrometry.

A selective and sensitive procedure has been developed and validated for the determination of acrylamide in difficult matrices, such as coffee and chocolate. The proposed method includes pressurised fluid extraction (PFE) with acetonitrile, florisil clean-up purification inside the PFE extraction cell and detection by liquid chromatography (LC) coupled to atmospheric pressure ionisation in positive mode tandem mass spectrometry (APCI-MS-MS). Comparison of ionisation sources (atmospheric pressure chemical ionisation (APCI), atmospheric pressure photoionization (APPI) and the combined APCI/APPI) and clean-up procedures were carried out to improve the analytical signal. The main parameters aff…

Determination of uranium in tap water by ICP-MS

A fast and accurate procedure has been developed for the determination of uranium at microg L(-1) level in tap and mineral water. The method is based on the direct introduction of samples, without any chemical pre-treatment, into an inductively coupled plasma mass spectrometer (ICP-MS). Uranium was determined at the mass number 238 using Rh as internal standard. The method provides a limit of detection of 2 ng L(-1) and a good repeatability with relative standard deviation values (RSD) about 3% for five independent analyses of samples containing 73 microg L(-1) of uranium. Recovery percentage values found for the determination of uranium in spiked natural samples varied between 91% and 106%…

Ceramic productions and human interactions during the Early Bronze Age in northern Iberia

The Early Bronze Age ceramic collection found into the caves of La Llana and El Toral III in Asturias (Spain) presents common decoration such as that found in the centre of Cantabrian Spain from the same period, which resembles others found in the Ebro Valley and Atlantic Europe. Therefore, the main objective of this study it is to identify the raw material origin and understand the pottery production process during the Early Bronze Age in the Cantabrian region. A methodological approach based on the chemical and mineralogical analysis of vessels and experimentally fired clay samples collected all over the centre of this region was developed. Furthermore, the post-depositional processes aff…

Sampling and analysis of pesticides in ambient air.

Developments in the sampling and determination of pesticides in ambient air have been discussed and data on the occurrence of pesticides in atmosphere have been presented. Developments in active sampling methods were reviewed and the different materials used for trapping pesticides from gas and particulate phases were discussed. Likewise, the use and developments of passive air samplers were reviewed. This article pays special attention to the analysis of pesticides trapped from ambient air, and recapitulate the procedures for extraction, clean-up and determination of these substances. Improvements in sampling procedures, analytical methods and monitoring activities are necessary to advance…

Passive Sampling of Atmospheric Organic Contaminants

The state of the art of passive sampling monitoring studies of atmospheric contaminants is reviewed in this chapter. The following passive samplers were considered: badge-type diffusive samplers; diffusive tubes; semi-permeable membrane devices; Radiello samplers; solid-phase microextraction fibers; polyurethane foam disks; XAD-2 passive air samplers; stir-bar samplers; polymer-coated glass surfaces; versatile, easy and rapid atmospheric monitor; and vegetation. A summary of the passive samplers used, sampling times, sampling rates, and analyte concentrations found is provided for different organic compounds, such as: carbonyl compounds, volatile compounds, polycyclic aromatic hydrocarbons,…