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1.
Marta Pedrouzo Francesc Borrull Rosa Maria Marcé Eva Pocurull 《Analytical and bioanalytical chemistry》2010,397(7):2833-2839
Stir-bar-sorptive extraction (SBSE) with liquid desorption (LD) and ultra-high-performance liquid chromatography–electrospray
ionization triple-quadrupole tandem mass spectrometry (UHPLC–(ESI)MS–MS) were used for analysis of six personal care products
in environmental water: four UV filters (2,2-dihydroxy-4-methoxybenzophenone, benzophenone-3, octocrylene, and octyldimethyl-p-aminobenzoic acid) and two antimicrobial agents (triclocarban and triclosan). Experimental conditions that affect SBSE-LD
sorption efficiency (extraction time and temperature, sample pH, and ionic strength) and desorption efficiency (solvent, temperature,
and time) were optimized. The method proved to be sensitive—a 50-mL sample was used to determine these compounds in environmental
waters at trace levels. The detection limits of the analytical method were 2.5 ng L−1 for river water and 5–10 ng L−1 for effluent and influent sewage water. In river waters, benzophenone-3 was found at levels from 6 ng L−1 to 28 ng L−1 and triclosan at levels <LOQ. Benzophenone-3 was found between 75 and 127 ng L−1 in influent sewage, whereas concentrations of benzophenone-3 and triclosan were commonly below 25 ng L−1 in effluent sewage. 相似文献
2.
A survey of contamination of surface and drinking waters around Lake Maggiore in Northern Italy with polar anthropogenic environmental
pollutants has been conducted. The target analytes were polar herbicides, pharmaceuticals (including antibiotics), steroid
estrogens, perfluorooctanesulfonate (PFOS), perfluoroalkyl carboxylates (including perfluorooctanoate PFOA), nonylphenol and
its carboxylates and ethoxylates (NPEO surfactants), and triclosan, a bactericide used in personal-care products. Analysis
of water samples was performed by solid-phase extraction (SPE) then liquid chromatography–triple-quadrupole (tandem) mass
spectrometry (LC–MS–MS). By extraction of 1-L water samples and concentration of the extract to 100 μL, method detection limits
(MDLs) as low as 0.05–0.1 ng L−1 were achieved for most compounds. Lake-water samples from seven different locations in the Southern part of Lake Maggiore
and eleven samples from different tributary rivers and creeks were investigated. Rain water was also analyzed to investigate
atmospheric input of the contaminants. Compounds regularly detected at very low concentrations in the lake water included:
caffeine (max. concentration 124 ng L−1), the herbicides terbutylazine (7 ng L−1), atrazine (5 ng L−1), simazine (16 ng L−1), diuron (11 ng L−1), and atrazine-desethyl (11 ng L−1), the pharmaceuticals carbamazepine (9 ng L−1), sulfamethoxazole (10 ng L−1), gemfibrozil (1.7 ng L−1), and benzafibrate (1.2 ng L−1), the surfactant metabolite nonylphenol (15 ng L−1), its carboxylates (NPE1C 120 ng L−1, NPE2C 7 ng L−1, NPE3C 15 ng L−1) and ethoxylates (NPE
n
Os, n = 3-17; 300 ng L−1), perfluorinated surfactants (PFOS 9 ng L−1, PFOA 3 ng L−1), and estrone (0.4 ng L−1). Levels of these compounds in drinking water produced from Lake Maggiore were almost identical with those found in the lake
itself, revealing the poor performance of sand filtration and chlorination applied by the local waterworks. 相似文献
3.
Manuela Haunschmidt Christian W. Klampfl Wolfgang Buchberger Robert Hertsens 《Analytical and bioanalytical chemistry》2010,397(1):269-275
A screening method for analyzing environmental waters contaminated with UV filters using direct analysis in real-time mass
spectrometry (DART-MS) was developed. To demonstrate the suitability of DART-MS a test set of seven organic UV filters, namely
benzophenone-3 (BP-3), ethylhexyl dimethyl p-aminobenzoate (OD-PABA), 4-t-butyl-4′-methoxydibenzoylmethane (BM-DBM), homomethyl salicylate (HMS), 2-(ethylhexyl) salicylate (EHS), octocrylene (OC),
and 4-methylbenzylidene camphor (4-MBC), was defined. In the first step, standard solutions of the analytes prepared in methanol
were investigated in order to determine optimum parameters for the DART-MS. Because of the very low concentrations of UV filters
expected in environmental water samples, a pre-concentration step using stir bar sorptive extraction was performed. DART-MS
allows the direct, simple and rapid semi-quantitative analysis of the analytes enriched on the surface of the polydimethylsiloxane-coated
stir bars. The optimized method provided calibration curves with correlation coefficients R > 0.959, repeatability from 5% (for 4-MBC) to 30% (for BM-DBM) relative standard deviation and limits of detection lower
than 40 ng L−1 for all analytes. Finally, real lake water samples from locations with typical leisure activities were analyzed. Results
obtained with the developed DART-MS method were cross-checked by confirmatory analysis using thermodesorption gas chromatography
mass spectrometry (TD-GC-MS). Thereby, it could be demonstrated that both analytical methods provide comparable concentrations
for the UV filters in the lake water samples. 相似文献
4.
León Z Balaguer A Chisvert A Salvador A Herráez M Díez O 《Analytical and bioanalytical chemistry》2008,391(3):859-866
An analytical method based on ion-interaction chromatography with UV detection for simultaneous in-vitro estimation of the
percutaneous absorption of the most used water-soluble UV filters in sunscreen cosmetics is proposed. These UV filters were
phenylbenzimidazole sulfonic acid, disodium phenyl dibenzimidazole tetrasulfonate, benzophenone-4, and terephthalylidene dicamphor
sulfonic acid. The methodology is based on applying the sunscreen containing the target UV filters to human epidermis in a
diffusion cell. Analytes are determined in the receptor solution. To ensure skin integrity, screening of the cells was carried
out by analytical determination of a marker. Analytical variables such as percentage ethanol, concentration of ion-pairing
agent, pH of the mobile phase, and temperature were studied in order to achieve high resolution of the chromatographic peaks
in the lowest possible time of analysis. The conditions selected consisted of a mobile phase composed of 35:65 (v/v) ethanol–ammonium acetate buffer solution (pH 4, containing 50 mmol L−1 tetra-n-butylammonium bromide). The chromatographic determination was carried out with the analytical column at 50 °C. UV detection
was carried out at the maximum absorption wavelength for each analyte. The limit of detection (3s
y/x
/b) ranged from 16 to 65 ng mL−1, depending on the analyte. 相似文献
5.
Popp M Hann S Mentler A Fuerhacker M Stingeder G Koellensperger G 《Analytical and bioanalytical chemistry》2008,391(2):695-699
A novel method employing high-performance cation chromatography in combination with inductively coupled plasma dynamic reaction
cell mass spectrometry (ICP–DRC–MS) for the simultaneous determination of the herbicide glyphosate (N-phosphonomethylglycine) and its main metabolite aminomethyl phosphonic acid (AMPA) is presented. P was measured as 31P16O+ using oxygen as reaction gas. For monitoring the stringent target value of 0.1 μg L−1 for glyphosate, applicable for drinking and surface water within the EU, a two-step enrichment procedure employing Chelex
100 and AG1-X8 resins was applied prior to HPIC–ICP–MS analysis. The presented approach was validated for surface water, revealing
concentrations of 0.67 μg L−1 glyphosate and 2.8 μg L−1 AMPA in selected Austrian river water samples. Moreover, investigations at three waste water-treatment plants showed that
elimination of the compounds at the present concentration levels was not straightforward. On the contrary, all investigated
plant effluents showed significant amounts of both compounds. Concentration levels ranged from 0.5–2 μg L−1 and 4–14 μg L−1 for glyphosate and AMPA, respectively. 相似文献
6.
Ru-Song Zhao Xia Wang Jing Sun Shan-Shan Wang Jin-Peng Yuan Xi-Kui Wang 《Analytical and bioanalytical chemistry》2010,397(4):1627-1633
A novel and environmentally friendly microextraction method, termed ionic liquid dispersive liquid-phase microextraction (IL-DLPME),
has been developed for rapid enrichment of triclosan and triclocarban before analysis by high-performance liquid phase chromatography–electrospray
tandem mass spectrometry (HPLC–ESI-MS–MS). Instead of using toxic organic solvents, an ionic liquid was used as a green extraction
solvent. This also avoided the instability of the suspending drop in single-drop liquid-phase microextraction, and the heating
and cooling step in temperature-controlled ionic liquid dispersive liquid phase microextraction. Factors that may affect the
enrichment efficiency, for example volume of ionic liquid, type and volume of dispersive solvent, pH, extraction time, and
NaCl content were investigated in detail and optimized. Under optimum conditions, linearity of the method was observed over
the range 0.2–12 μg L−1 for triclocarban and 1–60 μg L−1 for triclosan with correlation coefficients ranging from 0.9980 to 0.9990, respectively. The sensitivity of the proposed
method was found to be excellent, with limits of detection in the range 0.040–0.58 μg L−1 and precision in the range 7.0–8.8% (RSD, n = 5). This method has been successfully used to analyze real environmental water samples and satisfactory results were achieved.
Average recoveries of spiked compounds were in the range 70.0–103.5%. All these results indicated that the developed method
would be a green method for rapid determination of triclosan and triclocarban at trace levels in environmental water samples. 相似文献
7.
A simple and reliable method has been established for determination of cis and trans-1,3-dichloropropene (1,3-DCP) in water by headspace solid-phase microextraction (HS-SPME) then GC–ECD. An experimental design
with two steps was performed to determine the best experimental conditions for extraction of the 1,3-DCP isomers. First, a
26−2 fractional factorial design was conducted to screen for significant conditions. Second, a central composite design (CCD)
was performed to optimise the variables. The best experimental extraction conditions were: polydimethylsiloxane–divinylbenzene
(PDMS–DVB)-coated fibre, 20-min extraction time, 12 °C extraction temperature, 300 g L−1 NaCl, and 20 mL headspace volume in 40-mL vial. Under these conditions the method detection limit (MDL) was 0.5 ng L−1 for cis-1,3-DCP and 1.0 ng L−1 for trans-1,3-DCP. The method quantification limit (MQL) was 1.2 ng L−1 for cis-1,3-DCP and 3.0 ng L−1 for trans-1,3-DCP. For both isomers the relative standard deviation (RSD) for analysis of 50 ng L−1 or 0.5 μg L−1 of the isomer mixture was less than 8%. When the proposed method was applied to surface (river) water and tapwater samples
from Gipuzkoa province (Spain) the target analytes were not detected. The method was also used to investigate the presence
of the isomers in leachates from agricultural soil. A mixed solution was added to samples of two different soils and 1,3-DCP
isomers were quantified in leachate obtained from the samples. 相似文献
8.
Dolores Barranco Martínez María Martínez Galera Piedad Parrilla Vázquez M. Dolores Gil García 《Chromatographia》2007,66(7-8):533-538
Liquid chromatography with electrospray mass spectrometry (LC–ESI-MS) instrumentation equipped with a single quadrupole mass
filter has been used to determine several benzoylphenylurea insecticides (diflubenzuron, triflumuron, hexaflumuron, lufenuron
and flufenoxuron). Chromatographic and MS parameters were optimised to obtain the best sensitivity and selectivity for all
pesticides. Solid-phase extraction (SPE) using C18 cartridges was applied for preconcentration of pesticide trace levels in river water samples. Recoveries of benzoylphenylurea
pesticides from spiked river water (0.01 and 0.025 μg L−1) were between 73 and 110% and detection limits were between 3.5 and 7.5 ng L−1. The applicability of the method to the determination of benzoylphenylurea insecticides in spiked cucumber, green beans,
tomatoes and aubergines was evaluated. Samples were extracted into dichloromethane without any clean-up step. The limits of
detection ranged from 1.0 to 3.2 ng mL−1 (0.68 and 2.13 μg kg−1 in the vegetable samples). Mean recoveries ranged from 79 to 114% at spiking levels of 0.01 and 0.03 mg kg−1. The method was applied to determine traces of benzoylphenylureas in both river water and vegetable samples with precision
values lower than 10%. Interferences due to the matrix effect were overcome using matrix-matched standards. 相似文献
9.
Montesdeoca-Esponda S Sosa-Ferrera Z Santana-Rodríguez JJ 《Analytical and bioanalytical chemistry》2012,403(3):867-876
Benzotriazoles are a group of UV absorbing compounds considered emerging contaminants that are used in different personal
care products, and therefore, it is of high interest to develop sensitive and fast methods for investigating their presence
in the environment. In this work, we present the development and application of a novel method based on on-line solid-phase
extraction coupled to ultra-performance liquid chromatography with tandem mass spectrometry detection (SPE-UPLC-MS/MS) for
the determination of seven benzotriazole UV stabilizers (BUVSs) in coastal marine and wastewater samples. This process is
compared with a conventional off-line SPE procedure followed by UPLC-MS/MS. The parameters affecting the performance of the
sample preparation and determination processes were evaluated. The results indicate that the on-line procedure provides for
better sensitivity and reproducibility and is faster and easier than the off-line procedure. The detection limits and quantification
limits achieved were in the range of 0.6–4.1 ng∙L−1 and 2.1–14 ng∙L−1 and relative standard deviation between 6.2 and 10 %. The developed method was applied to coastal marine and wastewater samples
from Gran Canaria Island (Spain). All of the BUVSs studied were detected in the samples from wastewater treatment plants and
two were found in the seawater samples (UV P in the range of 2.8–4.4 ng∙L−1 and UV 360 between 3.6 and 5.2 ng∙L−1). 相似文献
10.
Continuous disposal of endocrine-disrupting compounds (EDCs) into the environment can lead to serious human health problems
and can affect plants and aquatic organisms. The determination of EDCs in water has become an increasingly important activity
due to our increased knowledge about their toxicities, even at low concentration. The EDCs in water samples from the reclaimed
water plant of Tianjin, northern China, were identified by gas chromatography (GC)–mass spectrometry (MS). Important and contrasting
EDCs including estrone (E1), 17β-estradiol (E2), 17α-ethynylestradiol (EE2), 4-tert-octylphenol (OP), 4-nonylphenol (NP),
bisphenol A (BPA), di-n-butyl phthalate (DnBP), diisobutyl phthalate (DIBP), and di(2-ethylhexyl)phthalate (DEHP) were selected as the target compounds.
Concentrations of steroid hormones, alkylphenolic compounds and phthalates ranged from below the limit of detection (LOD)
to 8.1 ng L−1, from <LOD to 14.2 ng L−1, and from 1.00 μg L−1 to 23.8 μg L−1, respectively. The average removal efficiencies for target EDCs varied from 30% to 82%. These results indicate that environmental
endocrine disrupting compounds are not completely removed during reclaimed water treatment and may be carried over into the
general aquatic environment. 相似文献
11.
Perreau F Bados P Kerhoas L Nélieu S Einhorn J 《Analytical and bioanalytical chemistry》2007,388(5-6):1265-1273
Two alternatives for the rapid simultaneous quantification of six sulfonylurea herbicides and five of their main degradation
products in natural water are proposed. For concentration, the compounds were extracted on a polystyrene–divinylbenzene solid
phase under pH and elution conditions that suppressed any hydrolysis. The eluates were analysed by liquid chromatography coupled
to electrospray tandem mass spectrometry within 20 min. The whole method was validated and shown to give no hydrolysis artefacts.
The application of off-line and on-line SPE of sulfonylureas enabled the 0.1 μg L−1 and 1 ng L−1 LOQ levels to be reached, respectively. The on-line SPE–LC–MS–MS method allowed the accurate quantitation of all sulfonylureas
and three degradation products at 0.1 μg L−1 or below in natural water, with an average repeatability of 8%. 相似文献
12.
Chromatography-mass spectrometry and toxicity evaluation of selected contaminants in seawater 总被引:1,自引:0,他引:1
M. Mezcua M. D. Hernando L. Piedra A. Agüera A. R. Fernández-Alba 《Chromatographia》2002,56(3-4):199-206
Summary In the present work a combined analytical study involving gas and liquid-chromatography and toxicity studies were developed
for the determination of various contaminants typically present in sea water samples. The compounds investigated were Diuron,
Chlorothalonil, Dichlofluanid, TCMTB (2-thiocyanomethylthiobenzothiazole), lrgarol 1051, Sea nine 211 and MTBE (methyl-tert-butyl
ether). The selected compounds are additives of boat paints and gasoline and they can release into the aquatic environment
in considerable amounts in areas with intense shipping traffic. The developed analytical protocol consisted on the use of
a solid phase extraction procedure with Oasis™ HLB cartridges followed by GC-El/NCI-MS and LC-ES-MS both in SIM mode. Average recoveries, loading 600 mL of samples with
pH=3, varied from 40 to 95% and the detection limits ranged from 1–25 ng L−1. The developed method was applied to real samples from various marinas of Andalusia (Spain).Daphnia magna, Vibrio fischeri andSelenastrum capricornotum toxicity bioassays on individual and mixtures of selected compounds were applied to evaluate EC50 (effective concentration) and LOEC (lowest observable effect concentration) values. Resulting values were in the range of
0.001–720 mg L−1 for EC50 and 0.8.10−9–30 mg L−1 for LOEC for all contaminants except for MTBE where no toxic effect were found up to 680 mg L−1 onDaphnia magna. Toxicity effects of binary mixtures of the selected compounds showed synergistic effects in the majority of the cases (47.6%)
and antagonistic in the lower of the cases (9.5%). Levels of the contaminants found in the seawater samples showed around
a 30% of inhibition on tested species, during the summer months considering mixture lrgarol 1051-Diuron. Accelerated toxicity
processes were observed in mixtures MTBE-Diuron and MTBE-Dichlofluanid.
Presented in the Workshop “GPoll of European Science Foundation” Barcelona, Spain, 8–10 November 2001. 相似文献
13.
A fully automated method using direct immersion solid-phase microextraction (DI-SPME) and headspace on-fiber silylation for
simultaneous determinations of exogenous endocrine-disrupting chemicals (EDCs) and endogenous steroid hormones in environmental
aqueous and biological samples by gas chromatography–mass spectrometry (GC-MS) was developed and compared to a previously
reported manual method. Three EDCs and five endocrine steroid hormones were selected to evaluate this method. The extraction
and derivatization time, ion strength, pH, incubation temperature, sample volume, and extraction solvent were optimized. Satisfactory
results in pure water were obtained in terms of linearity of calibration curve (R
2=0.9932–1.0000), dynamic range (3 orders of magnitude), precision (4–9% RSD), as well as LOD (0.001–0.124 μg L−1) and LOQ (0.004–0.413 μg L−1), respectively. These results were similar to those obtained using a manual method, and moreover, the precision was improved.
This new automated method has been applied to the determinations of target compounds in real samples used in our previous
study on a manual SPME method. Exogenous octylphenol (OP), technical grade nonylphenol (t-NP), and diethylstilbestrol (DES) were at 0.13, 5.03, and 0.02 μg L−1 in river water and 3.76, 13.25, and 0.10 μg L−1 in fish serum, respectively. Natural steroid hormones estrone (E1), 17β-estradiol (E2), and testosterone (T) were at 0.19, 0.11, and 6.22 μg L−1 in river water; and in female fish serum E1, E2, and pregnenolone (PREG) were at 1.37, 1.95, and 6.25 μg L−1, respectively. These results were confirmed by the manual method. The developed fully automated SPME and on-fiber silylation
procedures showed satisfactory applications in environmental analysis and the performances show improved precision and a reduced
analysis time compared to the manual method. 相似文献
14.
N. Negreira I. Rodríguez E. Rubí R. Cela 《Analytical and bioanalytical chemistry》2010,398(2):995-1004
The performance of the dispersive liquid–liquid microextraction (DLLME) technique for the determination of eight UV filters
and a structurally related personal care species, benzyl salicylate (BzS), in environmental water samples is evaluated. After
extraction, analytes were determined by gas chromatography combined with mass spectrometry detection (GC-MS). Parameters potentially
affecting the performance of the sample preparation method (sample pH, ionic strength, type and volume of dispersant and extractant
solvents) were systematically investigated using both multi- and univariant optimization strategies. Under final working conditions,
analytes were extracted from 10 mL water samples by addition of 1 mL of acetone (dispersant) containing 60 μL of chlorobenzene
(extractant), without modifying either the pH or the ionic strength of the sample. Limits of quantification (LOQs) between
2 and 14 ng L−1, inter-day variability (evaluated with relative standard deviations, RSDs) from 9% to 14% and good linearity up to concentrations
of 10,000 ng L−1 were obtained. Moreover, the efficiency of the extraction was scarcely affected by the type of water sample. With the only
exception of 2-ethylhexyl-p-dimethylaminobenzoate (EHPABA), compounds were found in environmental water samples at concentrations between 6 ± 1 ng L−1 and 26 ± 2 ng mL−1. 相似文献
15.
A rapid, sensitive and environmentally friendly method for the analysis of 14 anilines in water samples by dispersive liquid–liquid
microextraction based on solidification of floating organic drop (DLLME-SFO) prior to gas chromatography–mass spectrometry
(GC-MS) was developed and optimized. In the proposed method, cyclohexane was used as the extraction solvent as its toxicity
was much lower than that of the solvent usually used in dispersive liquid–liquid microextraction (DLLME). In the optimized
conditions, the method exhibited good analytical performance. Based on a signal-to-noise ratio of 3, limits of detection for
anilines were in the range of 0.07 to 0.29 μg L−1, and the linear range was 0.5–200 μg L−1 with regression coefficients (r
2) higher than 0.9977. It was efficient for qualitative and quantitative analysis of anilines in water samples. The relative
standard deviations varied from 2.9 to 8.6 % depending on different compounds indicating good precision. Tap water and river
water were selected for evaluating the application to real water samples. The relative recoveries of anilines for the two
real samples spiked with 10 μg L−1 anilines were in the scope of 78.2–114.6 % and 77.3–115.6 %, respectively. 相似文献
16.
This study investigates an off-line solid phase extraction (SPE) for improving the sensitivity in the capillary electrophoretic
(CE) analysis of four cephalosporins. Two sorbents—LiChrolut-C18 and Oasis HLB—were used in a SPE process to detect cephalosporins in natural waters (tap, river and hospital sewage) and
their performances were compared. By using Oasis HLB sorbent higher recoveries for river water were obtained (94–107% when
500 mL of sample were analyzed). The off-line SPE–CZE method was validated for river water with good detection limits (3 μg L−1) and the linearity ranged between 5 and 200 μg L−1. 相似文献
17.
Summary The eleven priority, EPA phenolic pollutants were determined by liquid chromatography followed by two detectors in series;
UV and electrochemical. Three different adsorbents, Envi-Carb (a carbon black) and two functionalized polymeric resins, Bond
Elut PPL and another synthesized in our laboratory with an ocarboxybenzoyl moiety, were compared for solid-phase extraction
(SPE) to detect lower concentrations of the eleven phenolics in natural waters. Higher recoveries were obtained using the
functionalized polymeric adsorbents compared with Envi-Carb. When real samples were analysed, the synthetic adsorbent gave
lower interference than Bond Elut PPL and phenol was determined at low levels with no humic and fulvic acid inter-ference
when Na2SO3 was added. The linearity range for most compounds in tap water was 0.05–20 μg L−1 and the limits of detection were <35 ng L−1. Repeatability and reproducibility between days for real samples spiked at 0.1 μg L−1, expressed as relative standard deviation, were <8% and 10%, respectively. 相似文献
18.
Alaa S. Amin 《Chemical Papers》2009,63(6):625-634
A simple, selective, highly sensitive and accurate procedure for the determination of trace amounts of copper has been developed
based on solid-phase spectrophotometry. Copper reacts with 5-(2-benzothiazolylazo)-8-hydroxyquinoline (BTAHQ) to give a complex
with high molar absorptivity (3.17 × 107 L mol−1 cm−1, 3.07 × 108 L mol−1 cm−1, 1.22 × 109 L mol−1 cm−1, and 1.80 × 109 L mol−1 cm−1), fixed on a Dowex 1-X8 type anion-exchange resin for 10 mL, 100 mL, 500 mL, and 1000 mL, respectively. The absorbance at
667 nm and 800 nm packed in a 1.0 mm cell was measured directly. Calibration is linear over the range 0.2–3.7 μg L−1 with RSD of < 1.28 % (n = 10). The detection and quantification limits of the 500 mL sample method are 79 ng L−1 and 260 ng L−1 when using 60 mg of Dowex 1-X8. For a 1000 mL sample, the detection and quantification limits are 67 ng L−1 and 220 ng L−1 using 60 mg of the exchanger. Increasing the sample volume can enhance the sensitivity. The proposed method was applied to
the determination of copper in different environmental water samples (tap, pit, spring, and river), food products (rice, corn
flour, and tea), and mushrooms, using the standard addition technique. 相似文献
19.
A. Gentili D. Perret S. Marchese R. Mastropasqua R. Curini A. Di Corcia 《Chromatographia》2002,56(1-2):25-32
Summary ‘Free’ steroidal estrogens have been identified as compounds possibly responsible for endocrine-disruption of aquatic fauna
populating rivers in which municipal sewage-treatment plants (STP) discharge their effluents. Natural and synthetic estrogens
are excreted, as glucuronides and sulfates, by man, in the urine but these are bioconverted back to the unconjugated forms
in wastewater discharges. For this reason we have developed a sensitive analytical procedure, without derivatization, for
identification and quantitation of conjugated and free estrogens in surface and waste waters. The hormones were extracted
and fractionated, by use of Carbograph cartridges, into neutral and acid fractions which were then analyzed by liquid chromatography-tandem
mass spectrometry. Recoveries were between 66 and 100% and limits of detection (LOD) between 15.0 and 0.003 ng L−1, depending on the compound and the water matrix. When this methodology was applied to real sewage and river water we could
measure the main free estrogens at ng L−1 levels. Among the conjugates we always observed the presence of estrone 3-sulfate (at levels between 8.0 and 0.5 ng L−1). 相似文献
20.
This paper presents the development of a fast and sensitive analytical method for the simultaneous determination of UV filters
and degradation products having quite different polarities (log Kow 2.19–6.88) in sediment, by means of pressurized liquid
extraction (PLE) with in-cell purification and analysis by ultra-performance liquid chromatography (UPLC) coupled to tandem
mass spectrometry (MS/MS). Analytes were simultaneously concentrated and purified by placing aluminium oxide as clean-up sorbent
in the extraction cell for a faster sample pre-treatment. Under optimized conditions, quantitative recoveries (only one compound
below 80%) and satisfactory precision (RSD, 5–15%) were obtained. Low limits of detection were achieved of 0.5–15 ng/g dry
weight (dw). The use of PLE extraction and purification and UPLC technology enabled all the compounds to be separated chromatographically
in less than 9 min, and with a total chromatographic analysis time of 18 min. This method significantly decreased the overall
time of analysis as compared to those of previously developed. Finally, the optimized methodology was applied to investigate
the occurrence of the target UV filters in sediment samples collected along the Ebro river basin (Spain). UV filters were
detected in 95% of the sediment samples analysed. Results revealed a widespread presence of octocrylene (OC), reaching concentrations
up to 24 × 102 ng/g dw, the highest reported so far. Ethylhexyl dimethyl PABA (OD-PABA) and benzophenone-3 (BP3) were also frequently detected
(60–65%), but at lower concentrations (4.4–27 ng/g dw). 4DHB (an estrogenic degradation product of BP3) was present in three
samples at concentrations between 12 and 21 ng/g dw. These results constitute the first data on the occurrence of OD-PABA
and 4DHB in sediments. 相似文献