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1.
Sci Total Environ ; 835: 155400, 2022 Aug 20.
Article in English | MEDLINE | ID: mdl-35469867

ABSTRACT

Considering how the impact of human activity in Antarctica is growing, the aim of this study was to conduct the first assessment of pharmaceuticals and personal care products (PPCPs), other emerging contaminants (ECs), and antibiotic resistance genes present in the western shore of the Admiralty Bay region of King George Island. In total, more than 170 substances were evaluated to assess the potential environmental risks they pose to the study area. The major evaluated source of pollutants in this study is discharged untreated wastewater. The highest PPCP concentrations in wastewater were found for naproxen (2653 ngL-1), diclofenac (747 ngL-1), ketoconazole (760 ngL-1), ibuprofen (477 ngL-1) and acetaminophen (332 ngL-1). Moreover, the concentrations of benzotriazole (6340 ngL-1) and caffeine (3310 ngL-1) were also high. The Risk Quotient values indicate that azole antifungals (ketoconazole), anti-inflammatories (diclofenac, ibuprofen) and stimulants (caffeine) are the main groups responsible for the highest toxic burden. In addition, antibiotic resistance genes integrons (int 1) and sulphonamide resistance genes (sul 1-2) were detected in wastewater and seawater. These results indicate that regular monitoring of PPCPs and other ECs is of great importance in this environment. Additionally, the following mitigation strategies are suggested: (1) to create a centralised record of the medications prescribed and consumed in situ (to improve knowledge of potential contaminants without analysis); (2) to use more environmentally friendly substitutes both for pharmaceuticals and personal care products when possible (limiting consumption at the source); and (3) to apply advanced systems for wastewater treatment before discharge to the recipient (end-of-pipe technologies as a final barrier).


Subject(s)
Cosmetics , Water Pollutants, Chemical , Caffeine/analysis , Cosmetics/analysis , Diclofenac , Environmental Monitoring/methods , Humans , Ibuprofen , Ketoconazole/analysis , Pharmaceutical Preparations , Wastewater/analysis , Water Pollutants, Chemical/analysis
2.
Molecules ; 27(1)2021 Dec 23.
Article in English | MEDLINE | ID: mdl-35011310

ABSTRACT

In 2017, the Swedish Environmental Protection Agency published a report on advanced wastewater treatment for the removal of pharmaceutical residues and stated that advanced treatment should be implemented where it will make the largest difference from an environmental perspective. However, the report also concluded that this need cannot be specified with existing data, but consideration must be made of local conditions. Two considerations are (1) the discharged amount of pharmaceutical into receiving water bodies and (2) the turnover of water in the recipient, where the highest risks are related to recipients with a low water turnover and low dilution. The current project comprised eight different WWTPs distributed throughout the entire County Skåne (Scania) in Sweden, with a population of ca. 1,300,000 persons. In total, 21 of 22 pharmaceuticals were analyzed according to the list proposed by the Swedish Medical Products Agency 2015. The results show that large amounts of pharmaceuticals are released from the WWTPs yearly to Scanian recipients. The total discharge of pharmaceuticals from the eight treatment plants adds up to 71 kg of these 21 substances alone, mainly comprising metoprolol, which is a drug that lowers blood pressure, and the analgesic drug diclofenac. Additionally, carbamazepine, losartan, naproxen and oxazepam were present in significant concentrations. These represented three illnesses that are very common: high blood pressure, inflammation/pain and depression/anxiety. The concentrations were generally in line with previous national Swedish screenings. It was estimated that, when one million cubic meters (1,000,000 m3) of wastewater is discharged, almost 4 kg of the 21 pharmaceuticals is released. The total volume wastewater release by the >90 WWTPs in Scania was estimated to 152,887,000 m3, which corresponded to 590 kg/year. The investigated 21 drugs cover only a small part of many hundred pharmaceuticals that are in use in Sweden. Thus, most likely, one or several tons of pharmaceuticals leak out to the Scanian recipients annually. The analysis of river samples shows that the dilution of wastewater is a key parameter in reducing concentrations. However, some locations have remarkably high concentrations, which occur when the volume wastewater is large in relation to the flow in the river. These kinds of regional results are of importance when selecting where advanced treatment should be prioritized in a first instance, as requested by the Swedish EPA.


Subject(s)
Pharmaceutical Preparations/analysis , Wastewater/analysis , Water Pollutants, Chemical/analysis , Water Purification/legislation & jurisprudence , Environmental Monitoring/legislation & jurisprudence , Environmental Monitoring/methods , Geography , Humans , Pharmaceutical Preparations/chemistry , Research , Rivers/chemistry , Sweden , Wastewater/chemistry , Water Pollutants, Chemical/chemistry , Water Purification/methods
3.
Molecules ; 24(7)2019 Apr 11.
Article in English | MEDLINE | ID: mdl-30978956

ABSTRACT

By using an innovative, positive pressure sample loading technique in combination with an in-line filter of finely ground sand the bottleneck of solid phase extraction (SPE) can be reduced. Recently published work by us has shown the proof of concept of the technique. In this work, emphasis is put on the SPE flow rate and method validation for 26 compounds of emerging environmental concern, mainly from the 1st and 2nd EU Watch List, with various physicochemical properties. The mean absolute recoveries in % and relative standard deviations (RSD) in % for the investigated compounds from spiked pure water samples at the three investigated flow rates of 10, 20, and 40 mL/min were 63.2% (3.2%), 66.9% (3.3%), and 69.0% (4.0%), respectively. All three flow rates produced highly repeatable results, and this allowed a flow rate increase of up to 40 mL/min for a 200 mg, 6 mL, reversed phase SPE cartridge without compromising the recoveries. This figure is more than four times the maximum flow rate recommended by manufacturers. It was indicated that some compounds, especially pronounced for the investigated macrolide molecules, might suffer when long contact times with the sample glass bottle occurs. A reduced contact time somewhat decreases this complication. A very good repeatability also held true for experiments on both spiked matrix-rich pond water (high and low concentrations) and recipient waters (river and wastewater) applying 40 mL/min. This work has shown that, for a large number of compounds of widely differing physicochemical properties, there is a generous flow rate window from 10 to 40 mL/min where sample loading can be conducted. A sample volume of 0.5 L, which at the recommended maximum flow rate speed of 10 mL/min, would previously take 50 min, can now be processed in 12 min using a flow rate of 40 mL/min. This saves 38 min per processed sample. This low-cost technology allows the sample to be transferred to the SPE-column, closer to the sample location and by the person taking the sample. This further means that only the sample cartridge would need to be sent to the laboratory, instead of the whole water sample, like today's procedure.


Subject(s)
Environmental Monitoring , Pesticides/chemistry , Water Pollutants, Chemical/chemistry , Chromatography, High Pressure Liquid , Fresh Water/chemistry , Humans , Pesticides/analysis , Pesticides/toxicity , Pressure , Rivers/chemistry , Silicon Dioxide/chemistry , Solid Phase Extraction , Tandem Mass Spectrometry , Water Pollutants, Chemical/isolation & purification
4.
J Pharm Biomed Anal ; 145: 569-575, 2017 Oct 25.
Article in English | MEDLINE | ID: mdl-28777968

ABSTRACT

This study demonstrates the addition of 14C-cholesterol to the human cell line H295R will in-situ form radiolabeled steroid hormones allowing for new mechanistic and metabolic insights. The aim of the present study was to in-situ radiolabel steroid hormones from cell line-incorporated 14C-cholesterol using the OECD guideline 456, H295R steroidogenesis in-vitro assay. Radiodetection of the steroid metabolites of the steroidogenic pathway allows for an improved understanding of the various enzymatic mechanisms involved without necessarily being dependent on quantification. Generated radiolabeled steroids were analyzed using HPLC hyphenated with a Flow Scintillation Analyzer (FSA). H295R cells were incubated with radiolabeled cholesterol and cell media were collected and prepared by solid phase extraction and analyzed with HPLC-FSA. For successful radiolabeling of the steroids in the steroidogenesis of H295R cells, radioactive cholesterol may potentially only need to be added just before the cells are incubated for 72h in well plates. Based on the obtained HPLC-FSA chromatograms, and confirmation of the observations by studies in the literature, a qualitative time profile for the production of steroid hormones was estimated. Multiple radiolabeled steroid hormones were identified by means of analytical standards and UV (ultraviolet) co-chromatography, though the elucidation of multiple metabolites remains unresolved. Although online radiodetection proved to suffer from suboptimal sensitivity, the concept of radiolabeling the steroidogenesis in H295R cells with 14C-cholesterol and detecting the radiolabeled steroid hormones online was proved and may assist in further toxicological studies.


Subject(s)
Adrenocortical Adenoma , Cell Line , Cell Line, Tumor , Cholesterol , Chromatography, High Pressure Liquid , Humans , Online Systems , Solid Phase Extraction , Steroids
5.
J Chromatogr B Analyt Technol Biomed Life Sci ; 1033-1034: 128-137, 2016 Oct 15.
Article in English | MEDLINE | ID: mdl-27543742

ABSTRACT

In this work the habitual behaviour of low pH in environmental organic trace analysis is challenged by investigating the full potential of building a multi-component UHPLC-ESI-MS/MS method adapted to cover common emerging contaminants of many different polarities, minimizing the elements of compromise in the performance of the final analytical separation and detection. Contributes have been made by taking advantage of common commercially available technology in understanding the impact from solvent components and the ionization of analytes which can facilitate future development of robust, sensitive and precise UHPLC-MS/MS methods. All contaminants were evaluated and optimized without prejudices regarding historical residence in terms of chromatographic conditions and ESI mode; increasing multi-method's flexibility that can be implemented in routine analysis in response to new requests as well as to emerging contaminants yet to be discovered. Our data strongly supports the questioning of the assumption that equilibrium concentrations of ions in solution reflect those produced during the electrospray process. ESI responses of [M+H](+) and limits of detection were comparable, or often better at high pH compared to acidic eluents. Presence of nitrogen basic groups such as tertiary and secondary amines in a compound increased the intensity of the ESI+ signal, and was even further elevated in basic eluent. The proton affinity probably changes for many nitrogen-containing compounds during the ionization process, making the gas-phase processes very important in generation of these ions by ESI+. There were also an unexpected large number of compounds showing their highest response at pH 7 and weak ionic strength. A flow optimized, buffert free, neutral UHPLC-MS/MS method enhanced the sensitivity for the environmental important synthetic hormone ethinyl estradiol significantly.


Subject(s)
Chromatography, High Pressure Liquid , Spectrometry, Mass, Electrospray Ionization , Tandem Mass Spectrometry , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/chemistry , Caffeine , Chromatography, High Pressure Liquid/instrumentation , Chromatography, High Pressure Liquid/methods , Chromatography, High Pressure Liquid/standards , Equipment Design , Ethinyl Estradiol , Hydrogen-Ion Concentration , Models, Theoretical , Nitrogen , Spectrometry, Mass, Electrospray Ionization/instrumentation , Spectrometry, Mass, Electrospray Ionization/methods , Spectrometry, Mass, Electrospray Ionization/standards , Tandem Mass Spectrometry/instrumentation , Tandem Mass Spectrometry/methods , Tandem Mass Spectrometry/standards
6.
Arch Environ Contam Toxicol ; 71(3): 423-36, 2016 Oct.
Article in English | MEDLINE | ID: mdl-27480162

ABSTRACT

This study is the first to investigate the pharmaceutical burden from point sources affecting the UNESCO Biosphere Reserve Kristianstads Vattenrike, Sweden. The investigated Biosphere Reserve is a >1000 km(2) wetland system with inflows from lakes, rivers, leachate from landfill, and wastewater-treatment plants (WWTPs). We analysed influent and treated wastewater, leachate water, lake, river, and wetland water alongside sediment for six model pharmaceuticals. The two WWTPs investigated released pharmaceutical residues at levels close to those previously observed in Swedish monitoring exercises. Compound-dependent WWTP removal efficiencies ranging from 12 to 100 % for bendroflumethiazide, oxazepam, atenolol, carbamazepine, and diclofenac were observed. Surface-water concentrations in the most affected lake were ≥100 ng/L for the various pharmaceuticals with atenolol showing the highest levels (>300 ng/L). A small risk assessment showed that adverse single-substance toxicity on aquatic organisms within the UNESCO Biosphere Reserve is unlikely. However, the effects of combinations of a large number of known and unknown pharmaceuticals, metals, and nutrients are still unknown.


Subject(s)
Environmental Monitoring , Pharmaceutical Preparations/analysis , Water Pollutants, Chemical/analysis , Wetlands , Conservation of Natural Resources
7.
J Chromatogr B Analyt Technol Biomed Life Sci ; 1017-1018: 45-51, 2016 Apr 01.
Article in English | MEDLINE | ID: mdl-26945133

ABSTRACT

This paper presents the development and evaluation of a methodology for extraction, clean-up and analysis of three key corticosteroids (aldosterone, cortisol and corticosterone) in polar bear hair. Such a methodology can be used to monitor stress biomarkers in polar bears and may provide as a useful tool for long-term and retrospective information. We developed a combined pressurized liquid extraction (PLE)-solid phase extraction (SPE) procedure for corticosteroid extraction and clean-up followed by high pressure liquid chromatography tandem mass spectrometry (HPLC-MS/MS) analysis. This procedure allows for the simultaneous determination of multiple steroids, which is in contrast to previous polar bear studies based on ELISA techniques. Absolute method recoveries were 81%, 75% and 60% for cortisol, corticosterone and aldosterone, respectively. We applied the developed method on a hair sample pooled from four East Greenland polar bears. Herein cortisol and corticosterone were successfully determined in levels of 0.32±0.02ng/g hair and 0.13±0.02ng/g hair, respectively. Aldosterone was below limit of detection (LOD<0.17ng/g). The cortisol hair concentration found in these East Greenland polar bears was consistent with cortisol levels previously determined in the Southern Hudson Bay and James Bay in Canada using ELISA kits.


Subject(s)
Adrenal Cortex Hormones/analysis , Chromatography, High Pressure Liquid/methods , Hair/chemistry , Tandem Mass Spectrometry/methods , Animals , Solid Phase Extraction , Ursidae
8.
J Chromatogr A ; 1415: 73-82, 2015 Oct 09.
Article in English | MEDLINE | ID: mdl-26362805

ABSTRACT

Over the past 30 years a vast number of studies have demonstrated the presence of pharmaceutical residues in the environment. But still knowledge is scarce regarding the interaction of these emerging pollutants with various matrices in nature. A chromatographic system with on-line detection was developed to perform a sorption study of six selected pharmaceuticals to four natural sediments and dewatered digested sewage treatment plant sludge with differing physicochemical characteristics. Sorption effects, measured as asymmetry factors and recoveries, differed pronouncedly among the pharmaceuticals and between the matrices, which could be explained by basic physicochemical properties of the investigated compounds in relation to matrix characteristics. Protonated and deprotonated molecular properties had the greatest importance for sorbate-sorbent interactions. Atenolol, with cationic properties, showed the highest degree of sorption regardless of the matrix studied. Diclofenac and furosemide, both acids, showed the least tendency towards interactions to natural matrices. Among the neutral compounds bendroflumethiazide, carbamazepine and oxazepam, weaker forces, such as van der Waals, aromatic electron donor-acceptor interactions, and hydrogen forces, seemed more important to determine sorption differences. Results revealed that sorption of pharmaceuticals on natural sediments decreased in the order: atenolol (+)>bendroflumethiazide>oxazepam>carbamazepine>diclofenac (-)>furosemide (-). The matrix content of organic matter measured as total organic carbon (TOC) clearly dictated drug sorption. Beside from studying matrix interaction, these results and the developed technique and methodology might find use in the development of new removal processes of pharmaceuticals from wastewater based on improved knowledge concerning chemical interactions to filter materials.


Subject(s)
Geologic Sediments/chemistry , Pharmaceutical Preparations/chemistry , Sewage/chemistry , Water Pollutants, Chemical/chemistry , Chromatography, Liquid , Lakes , Rivers , Sweden , United Nations , Wastewater
9.
Int J Toxicol ; 34(6): 534-42, 2015.
Article in English | MEDLINE | ID: mdl-26268768

ABSTRACT

Mixture effects of 3 model endocrine disruptors, prochloraz, ketoconazole, and genistein, on steroidogenesis were tested in the adrenocortical H295R cell line. Seven key steroid hormones (pregnenolone, progesterone, dehydroepiandrosterone, androstenedione, testosterone, estrone, and 17ß-estradiol) were analyzed using gas chromatography and tandem mass spectrometry (GC-MS/MS) to investigate the effects throughout the steroidogenic pathway. Current modeling approaches often rely on models assuming compounds acting independently and that the individual effects in some way can be summarized to predict a mixture effect. In H295R cells with an intact steroidogenic pathway, such assumptions may not be feasible. The purpose of this study was therefore to evaluate whether effects of a mixture with differing modes of action followed or deviated from additivity (concentration addition) and whether the H295R cell line was suitable for evaluating mixture toxicity of endocrine disruptors with different modes of action. The compounds were chosen because they interfere with steroidogenesis in different ways. They all individually decrease the concentrations of the main sex steroids downstream but exert different effects upstream in the steroidogenic pathway. Throughout the study, we observed lowest observed effect concentrations of mixtures at levels 2 to 10 times higher than the predicted EC(50), strongly indicating antagonistic effects. The results demonstrate that chemical analysis combined with the H295R cell assay is a useful tool also for studying how mixtures of endocrine disruptors with differing modes of action interfere with the steroidogenic pathway and that existing models like concentration addition are insufficient in such cases. Furthermore, for end points where compounds exert opposite effects, no relevant models are available.


Subject(s)
Endocrine Disruptors/toxicity , Genistein/toxicity , Imidazoles/toxicity , Ketoconazole/toxicity , Steroids/biosynthesis , Cell Line, Tumor , Cell Survival/drug effects , Drug Interactions , Humans
10.
Conserv Physiol ; 3(1): cov016, 2015.
Article in English | MEDLINE | ID: mdl-27293701

ABSTRACT

We developed a chemical analytical procedure for sampling, extracting and determining epidermal skin cortisol concentrations (SCCs) in the harbour porpoise (Phocoena phocoena) using gas chromatography-tandem mass spectrometry. In brief, this involved a pressurized liquid extraction with a two-step solid-phase clean-up. A derivatization step was conducted prior to detection. To evaluate the new assay, cortisol was analysed in three different sample types obtained from four harbour porpoises: skin plates, dorsal fin skin plugs (with and without lidocaine) and epidermal scrapes. Skin cortisol concentrations could be measured using the new assay in the majority of the tested skin samples down to a minimal sample size of 49 mg dry weight (dw). Water content ranged from 10 to 46% in the plug samples, which had SCCs from 2.1 to 77.7 ng/g dw. Epidermal scrape samples had the highest water content (83-87%) and lower SCCs (0.6-15 ng/g dw), while the skin plates had intermediate water contents (60-66%) and SCCs of 2.6-13.0 ng/g dw. SCC was slightly higher in plugs with lidocaine than without (average values of 41 and 33 ng/g dw, respectively). Substantial within-individual variations in cortisol concentrations are also common in other matrices such as blood and hair. Some important factors behind this variation could be e.g. the animal's sex, age, body condition, reproductive stage, and the body region sampled, as well as season, moulting cycles and water temperature. Clearly, more research into SCCs is required. The findings described here represent the first critical steps towards using epidermal skin cell samples to assess chronic stress levels in cetaceans and the development of a widely applicable health-assessment tool in these species.

11.
Article in English | MEDLINE | ID: mdl-24911547

ABSTRACT

Antimalarial drugs commonly referred to as antimalarials, include a variety of compounds with different physicochemical properties. There is a lack of information on antimalarial distribution in the body over time after administration, e.g. the drug concentrations in whole blood, plasma, and urine, which must be improved in order to advance curing the parasitic disease malaria. A key problem also lies in that pharmacokinetic studies not always are performed in patient groups that may benefit most of the treatment such as children, pregnancy and lower-weight ethnic populations. Here we review the available sample preparation strategies combined with liquid chromatographic (LC) analysis to determine antimalarials in whole blood, plasma and urine published over the last decade. Sample preparation can be done by protein precipitation, solid-phase extraction, liquid-liquid extraction or dilution. After LC separation, the preferred detection tool is tandem mass spectrometry (MS/MS) but other detection methods have been used e.g. UV, fluorescence and electrochemical detection. Major trends for sample preparation of the different groups of antimalarials for each matrix and its detection have been summarized. Finally, the main problems that the researchers have dealt with are highlighted. This information will aid analytical chemists in the development of novel methods for determining existing antimalarials and upcoming new drugs.


Subject(s)
Antimalarials/blood , Antimalarials/urine , Drug Monitoring/methods , Antimalarials/chemistry , Chromatography, Liquid/methods , Dried Blood Spot Testing/methods , Humans , Liquid-Liquid Extraction/methods , Solid Phase Extraction/methods , Tandem Mass Spectrometry/methods
12.
Article in English | MEDLINE | ID: mdl-23948237

ABSTRACT

The H295R in vitro cell line produces the majority of the steroidogenesis, for which reason it is commonly used as a screening tool for endocrine disrupting chemicals. Simultaneous determination of the precursor cholesterol and key steroid hormones could give a broad insight into the mechanistic disruption of the steroidogenesis. Steroid hormones have primarily been extracted from H295R incubation medium by means of liquid-liquid extraction (LLE) and the obtained recoveries and matrix effects have typically not been stated or assessed. In the present study a solid-phase extraction (SPE) method was developed and validated for the simultaneous extraction of cholesterol and five key steroid hormones pregnenolone, 17-hydroxyprogesterone, testosterone, cortisol and aldosterone from H295R incubation medium, and finally detected by LC-MS/MS. Cholesterol was recovered at a level of 55.7%, while steroid hormone recoveries ranged from 98.2 to 109.4%. Matrix effects varied between -0.6% and 62.8%. Intra-day precision was deemed acceptable, but the inter-day precision for pregnenolone and aldosterone exceeded the precision limit of 15% RSD. Although LLE has been the most frequently used extraction method in H295R studies, however, our investigation has shown that SPE may relatively easily extract and recover steroid hormones, potentially replacing LLE.


Subject(s)
Chromatography, Liquid/methods , Solid Phase Extraction/methods , Steroids/analysis , Steroids/isolation & purification , Tandem Mass Spectrometry/methods , Cell Line, Tumor , Culture Media, Conditioned/chemistry , Culture Media, Conditioned/metabolism , Humans , Limit of Detection , Reproducibility of Results , Steroids/chemistry , Steroids/metabolism
13.
Environ Pollut ; 182: 177-83, 2013 Nov.
Article in English | MEDLINE | ID: mdl-23917220

ABSTRACT

Hydrolytic and photolytic degradation were investigated for the ionophore antibiotics lasalocid, monensin, salinomycin, and narasin. The hydrolysis study was carried out by dissolving the ionophores in solutions of pH 4, 7, and 9, followed by incubation at three temperatures of 6, 22, and 28 °C for maximum 34 days. Using LC-MS/MS for chemical analysis, lasalocid was not found to hydrolyse in any of the tested environments. Monensin, salinomycin, and narasin were all stable in neutral or alkaline solution but hydrolysed in the solution with a pH of 4. Half-lives at 25 °C were calculated to be 13, 0.6, and 0.7 days for monensin, salinomycin, and narasin, respectively. Absorbance spectra from each compound indicated that only lasalocid is degraded by photolysis (half-life below 1 h) due to an absorbance maximum around 303 nm, and monensin, salinomycin, and narasin are resistant to direct photolysis because they absorb light of environmentally irrelevant wavelengths.


Subject(s)
Anti-Bacterial Agents/chemistry , Ionophores/chemistry , Water Pollutants, Chemical/chemistry , Half-Life , Hydrogen-Ion Concentration , Lasalocid/chemistry , Models, Chemical , Monensin/chemistry , Photolysis , Pyrans/chemistry , Temperature
14.
J Chromatogr A ; 1307: 27-33, 2013 Sep 13.
Article in English | MEDLINE | ID: mdl-23890553

ABSTRACT

A multi-residue pressurised liquid extraction (PLE) methodology has been established for the determination of the four ionophores: lasalocid, monensin, salinomycin and narasin in solid environmental matrices. The PLE methodology is combined with solid phase extraction as clean-up using liquid chromatography coupled to tandem mass spectrometry applying electrospray ionisation for detection. The samples were freeze-dried prior to extraction. The absolute recoveries for soil and sediment ranged from 71 to 123% (relative standard deviation (RSDs) below 16%) and in the range 94-133% (RSDs 9-35%) for poultry manure. The final method allowed for the detection of four ionophores down to a few hundred ngkg(-1) in natural solid matrices with limit of quantifications (LOQs) being 0.96, 0.87, 0.98, and 0.64µgkg(-1) in soil for lasalocid, monensin, salinomycin, and narasin, respectively. Corresponding LOQs in sediment were 1.28, 1.34, 1.39, and 0.78µgkg(-1) for the respective ionophores, while in manure the LOQs were 0.98, 1.01, 1.45, and 1.01µgkg(-1).


Subject(s)
Environmental Pollutants/analysis , Ionophores/analysis , Liquid-Liquid Extraction/methods , Manure/analysis , Soil/chemistry , Animals , Chromatography, Liquid/methods , Coccidiostats/analysis , Coccidiostats/isolation & purification , Environmental Pollutants/isolation & purification , Geologic Sediments/chemistry , Ionophores/isolation & purification , Limit of Detection , Methanol/chemistry , Poultry , Reproducibility of Results , Tandem Mass Spectrometry/methods , Temperature , Veterinary Drugs/analysis , Veterinary Drugs/isolation & purification
15.
Environ Pollut ; 180: 368-71, 2013 Sep.
Article in English | MEDLINE | ID: mdl-23726145

ABSTRACT

In this study we evaluate and demonstrate the occurrence of nine natural and one synthetic steroid hormone, including estrogens, androgens and progestagens in biogas final digestate byproduct (digestion liquid) commonly used as an agricultural fertilizer. We investigated two biogas sites that utilize different anaerobic digestion technologies (mesophilic and thermophilic) from swine manure and other organic wastes. Individual hormone concentration levels were observed up to 1478 ng g(-1) dry weight or 22.5 mg kg(-1) N with estrone and progesterone reaching highest concentration levels. Evaluation of the potential environmental burden through the application in agriculture was also assessed on the basis of predicted environmental concentrations. This study indicates that the biogas digestion process does not completely remove steroid hormones from livestock manure and use of final digestate byproduct on croplands contributes to the environmental emission of hormones.


Subject(s)
Agriculture , Fertilizers/analysis , Hormones/analysis , Soil Pollutants/analysis , Animals , Biofuels , Crops, Agricultural/growth & development , Environmental Monitoring
16.
Article in English | MEDLINE | ID: mdl-23598050

ABSTRACT

Analytical methodologies based on liquid or gas chromatography coupled to tandem mass spectrometry for the simultaneous determination of two or more endogenous steroid hormones in human and animal plasma and serum has received increased attention the last few years. Especially in the clinical setting steroid profiling is of major importance in disease diagnostics. This paper discusses recent findings in such multi-steroid hormone procedures published from 2001 to 2012. The aim was to elucidate possible relationships between chosen analytical technique and the obtained analyte sensitivity for endogenous steroid hormones. By evaluating the success, at which the currently applied techniques have been utilized, more general knowledge on the field is provided. Furthermore the evaluation provides directions in which future studies may be interesting to conduct.


Subject(s)
Chromatography, Liquid/methods , Gas Chromatography-Mass Spectrometry/methods , Hormones/blood , Steroids/blood , Tandem Mass Spectrometry/methods , Animals , Humans
17.
Arch Environ Contam Toxicol ; 65(1): 56-66, 2013 Jul.
Article in English | MEDLINE | ID: mdl-23440447

ABSTRACT

This work determines the principal environmental pollution pathways of pharmaceuticals on the island of Mallorca (Spain). The evaluation was made on the basis of the quantification of pharmaceutical residues by liquid chromatography-tandem mass spectrometry in several environmental water samples, including wastewater-treatment plant effluents, municipal solid waste landfill leachates, groundwater (GW), and marine water. An overall set of 19 pharmaceuticals has been identified in the environment of the 27 human pharmaceuticals investigated in this study. WWTP effluents are the main source of discharge of the pharmaceuticals into the aquatic environment. The data indicate that reuse of treated domestic wastewater for irrigation (which supplies some 30 % of the total water demand in Mallorca) contributes to the contamination of GW. In addition, leaching from landfills is identified as another, but minor, possible source of introduction of pharmaceuticals to GW aquifers. Finally, WWTP effluents ending in the Mediterranean Sea, primarily highly urbanized coastal areas, cause pharmaceutical residues to occur in marine water bodies.


Subject(s)
Environmental Monitoring/methods , Pharmaceutical Preparations/analysis , Water Pollutants, Chemical/analysis , Chromatography, Liquid/methods , Groundwater/analysis , Solid Phase Extraction/methods , Solid Waste/analysis , Spain , Tandem Mass Spectrometry/methods , Waste Disposal, Fluid
18.
Anal Chim Acta ; 755: 69-76, 2012 Nov 28.
Article in English | MEDLINE | ID: mdl-23146396

ABSTRACT

This paper presents the development, optimization and validation of a LC-MS/MS methodology to determine the antiparasitic veterinary drug toltrazuril and its two main metabolites, toltrazuril sulfoxide and toltrazuril sulfone, in environmental surface water, soil and animal manure. Using solid phase extraction and selective pressurized liquid extraction with integrated clean-up, the analytical method allows for the determination of these compounds down to 0.06-0.13 ng L(-1) in water, 0.01-0.03 ng g(-1)dw in soil and 0.22-0.51 ng g(-1) dw in manure. The deuterated analog of toltrazuril was used as internal standard, and ensured method accuracy in the range 96-123% for water and 77-110% for soil samples. The developed method can also be applied to simultaneously determine steroid hormones in the solid samples. The antiparasitic drug and its metabolites were found in manure and soil up to 114 and 335 pg g(-1) dw, respectively. Little is known regarding the environmental fate and effects of these compounds; consequently more research is urgently needed.


Subject(s)
Chemistry Techniques, Analytical , Manure/analysis , Soil/chemistry , Triazines/chemistry , Water/chemistry , Antiparasitic Agents/chemistry , Antiparasitic Agents/metabolism , Calibration , Chromatography, High Pressure Liquid , Mass Spectrometry , Molecular Structure , Triazines/metabolism , Veterinary Drugs
19.
Toxicol In Vitro ; 26(2): 343-50, 2012 Mar.
Article in English | MEDLINE | ID: mdl-22198065

ABSTRACT

The effects of three model endocrine disruptors, prochloraz, ketoconazole and genistein on steroidogenesis were tested in the adrenocortical H295R cell line to demonstrate that a broader mechanistic understanding can be achieved in one assay by applying chemical analysis to the H295R assay. Seven key steroid hormones (pregnenolone, progesterone, dehydroepiandrosterone, androstenedione, testosterone, estrone and 17ß-estradiol) were analyzed using a novel and thoroughly validated GC-MS/MS method. In addition to the simultaneous quantification of 7 steroid hormones, the present method also negates the potential problems of cross-reactivity that can be encountered in some immunoassays. Although all 3 test compounds decrease the concentrations of the main sex steroids, the chemicals exerted different effects upstream in the pathway. Exposure to prochloraz resulted in increased hormone levels upstream of steroid 17 alpha-hydroxylase/17,20 lyase (P450c17) and decreases downstream. Ketoconazole inhibited the entire pathway, while exposure to genistein resulted in increased hormone levels upstream of 3-ß-hydroxysteroid dehydrogenase (3ß-HSD) and decreases downstream. The results demonstrate that chemical analysis combined with the H295R cell assay is an useful tool for studying the mechanisms by which endocrine disruptors interfere with the steroidogenic pathway.


Subject(s)
Endocrine Disruptors/pharmacology , Genistein/pharmacology , Gonadal Steroid Hormones/metabolism , Imidazoles/pharmacology , Ketoconazole/pharmacology , Steroids/metabolism , Biological Assay/methods , Cell Line, Tumor , Chromatography, Gas , Humans , Tandem Mass Spectrometry
20.
Chemosphere ; 86(2): 212-5, 2012 Jan.
Article in English | MEDLINE | ID: mdl-22047618

ABSTRACT

Two anticoccidial agents, salinomycin and robenidine, heavily used in the worldwide veterinary meat production, were investigated for their potential biotic degradation by cultured soil bacteria. The degradation-study was performed in lab-scale bio-reactors under aerobic and anaerobic conditions incubated for 200 h with a mixed culture of soil bacteria. Samples were analyzed by LC-MS/MS and potential transformation products were tentatively identified. Salinomycin was degraded under aerobic conditions and traces could be found after 200 h, however, seems more persistent under anaerobic conditions. Four transformation products of salinomycin were discovered. Robenidine was degraded under aerobic and anaerobic conditions, however, traces of robenidine were observed after 200 h. Five biotic transformation products of robenidine were discovered.


Subject(s)
Coccidiostats/metabolism , Soil Pollutants/metabolism , Biodegradation, Environmental , Bioreactors , Chromatography, High Pressure Liquid , Coccidiostats/analysis , Pyrans/analysis , Pyrans/metabolism , Robenidine/analysis , Robenidine/metabolism , Soil Microbiology , Soil Pollutants/analysis , Tandem Mass Spectrometry , Time Factors
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