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Contamination des eaux usées par les perturbateurs endocriniens - Protocole d'analyse et résultats pour le triclosan, le triclocarban et les parabènes
Abstract
Le triclosan (TCS), le triclocarban (TCC) et les parabènes (esters de l’acide para-hydrobenzoïque) sont
employés en tant qu’antiseptiques et agents conservateurs dans les produits de soins corporels. Leur usage génère des inquiétudes sur leur devenir et leur effet potentiel sur la faune et la flore. En effet, ils sont introduits dans le milieu récepteur principalement via les effluents des stations d’épuration (STEP) et les rejets urbains de temps de pluie. Un protocole analytique, permettant la détermination simultanée des deux bactéricides TCS et TCC et des six parabènes méthylparabène (MeP), éthylparabène (EtP), propylparabène (PrP), butylparabène (BuP), isobutylparabène (IsoBuP) et benzylparabène (BzP) dans la phase dissoute d’échantillons d’eaux usées en entrée de station d’épuration, a été validé – extraction sur phase solide (SPE) et analyse en chromatographie liquide ultra haute performance couplée à un spectromètre de masse en tandem (UPLC/MS/MS). Les rendements d’extraction, optimisés pour les eaux usées, sont compris entre 84 et 105 % suivant le composé. L’analyse sur la phase particulaire est en cours de validation. Les niveaux de concentration du TCS, du TCC et des parabènes ont été déterminés à l’occasion de quatre campagnes sur les effluents des cinq émissaires de la station d’épuration Seine aval, en région parisienne. Des échantillons moyens sur 24 heures ont été prélevés, proportionnellement au débit dans des flacons en plastique dont la nature a été testée. La concentration maximale retrouvée est de 21 423 ng/L, 4 735 ng/L, 3 886 ng/L, < limite de quantification (LQ), 221 ng/L et 1 236 ng/L pour le
MeP, EtP, PrP, BzP, IsoBuP et BuP, respectivement. Le TCS et le TCC ont été observés à des concentrations de 1 386 ng/L et < LQ, respectivement.
... Among the analytical techniques used to identify and quantify parabens in water samples, liquid chromatography (LC) has become one of the most widely used techniques for their determination[21– 23]due to its high sensitivity, specificity and that it is not limited by the non-volatility of parabens. However, gas chromatography (GC) offers better sensitivity and lower detection limits for complex sample investigations when used in combination with flame ionization detection (FID)[13], mass spectrometry (MS)[14,15]and triple quadrupole mass spectrometry (MS/MS)[24]. It is well known that the semi-polar nature of the analytes (Log K ow values from 1.67 to 3.0) requires their derivatization in order to reduce adsorption on the chromatographic column or thermal decomposition of the analytes in the injector port and improve the sensitivity as well as peak separation as a result. ...
... Most available analytical methods for determining parabens in environmental water samples require some pretreatment to obtain an extract enriched with all of the target analytes and as free as possible of other matrix components[10]. With the purpose of obtaining this extract from a water sample, numerous extraction techniques have been used including the following: magnetic solid phase extraction (MSPE)[11], solid phase extraction (SPE)[12], dispersive liquid– liquid microextraction (DLLME)[13], stir-bar sorptive extraction (SBSE)[14,15]and solid phase microextraction (SPME)[16], among others. The SPE technique is usually implemented by using a small column or cartridge containing an appropriate sorbent. ...
... V). Ces résultats sont en accord avec la littérature, et montrent que les composés les plus fréquemment retrouvés sont le MeP, l'EtP, le PrP et le BuP du fait de leur grande utilisation dans les produits cosmétiquesGonzález-Mariño et al., 2011). Les concentrations de ces composés peuvent atteindre 12,6 μg.L −1 dans la phase dissoute d'eau usées collectées en entrée de station. ...
For several years, environmental exogenous agents called endocrine disruptors (ED) , are thought to interfere with reproduction and development fonctions in many organisms . For the Protection of the Environment and human health, the Water Framework Directive establishes environmental quality standards (EQS) and limits the ranges of thirty-three substances and eight other pollutants in surface waters. Nevertheless, it does not yet take into account the effect of these priority substances on ecosystems and humans including endocrine disruption. More than endocrine disruptors specificity (dose response curve , mixtures effect etc. .. ) make the identification process more complex. This thesis focuses on the study of hormonal effects, the most commonly encountered, estrogen disruption using the yeast estrogen screen (YES) as diagnostic tool. This study focuses particularly on the north of Tunisia, where the impact of ED on development of Aphanius fasciatus . Some xenoestrogens such as cadmium and PAH products generated by local industry are partly implicated on observed skeletal deformities. In parallel, some xenoestrogens (including parabens) are detected in the waters of sewage treatment plants. Other chemicals such as textile and food dyes also have endocrine activities. Under the supervision of water quality, it is necessary to develop rapid tests to detect endocrine disrupter and supplement chemical analyzes. Some active substances on the endocrine system is poorly immunogenic, the research axis developed in this thesis focuses on a peptide affinity for detecting a fungi toxin, ochratoxin A.
... Les concentrations de ces composés peuvent atteindre 12,6 μg.L −1 dans la phase dissoute d'eau usées collectées en entrée de station (Andersen et al., 2007). Récemment, une étude menée dans les émissaires franciliens montre des concentrations de MeP atteignant des concentrations de 21 μg.L −1 (Geara-Matta et al., 2011). Au niveau des MES, les résultats sont moins homogènes entre les trois stations. ...
Triclosan (TCS) is an antimicrobial agent widely used in many personal care products. This study investigated the occurrence of TCS in effluents, biosolids and surface waters, and its fate in wastewater treatment plants (WWTPs). The aqueous concentrations of TCS in nineteen effluents from Australian WWTPs ranged from 23 ng/L to 434 ng/L with a median concentration of 108 ng/L, while its concentrations in nineteen biosolids ranged from 0.09 mg/kg to 16.79 mg/kg on dry weight basis with a median concentration of 2.32 mg/kg. The removal rates for TCS in five selected WWTPs were found to range between 72% and 93%. Biological degradation was believed to be the predominant removal mechanism for TCS in the WWTPs. However, adsorption onto sludge also played a significant role in the removal of TCS in the WWTPs. TCS at concentrations up to 75 ng/L was detected in surface waters (outfall, upstream, and downstream) from five rivers receiving effluent discharge from WWTPs. Preliminary risk assessment based on the worst-case scenario showed that the TCS concentrations in surface waters might lead to risks to aquatic organisms such as algae. Based on the TCS levels in the biosolids, application of biosolids on agricultural land may also cause adverse effects in the soil environment.
Personal care products (PCPs) are widely used emerging contaminants which can cause adverse environmental effects. This paper reports the development and validation of a method based on solid-phase extraction (SPE) and ultra-high-performance liquid chromatography-electrospray ionisation-tandem mass spectrometry (UHPLC-(ESI)MS-MS) for simultaneously determining eleven PCPs: 4 preservatives (methylparaben; ethylparaben; benzylparaben; propylparaben); 2 antimicrobial agents (triclocarban and triclosan) and 5 UV filters (2,4-dihydroxybenzophenone; 2,2-dihydroxy-4-methoxybenzophenone; benzophenone-3; octocrylene and octyldimethyl-p-aminobenzoic acid) in environmental waters in only 9 run minutes of chromatographic separation. The SPE was carried out with two polymeric cartridges (Oasis HLB and Bond Elut Plexa). The recoveries obtained with Bond Elut Plexa were between 69% and 101% for 500 mL of river waters, with the exception of octyldimethyl-p-aminobenzoic acid (46%). Limits of detection for 500 mL of river water were in the range of 1-5 ng/L. Oasis HLB was chosen for wastewater samples with recoveries between 38% and 92% (250 mL of effluents) and 36-89% (100mL of influents). In both wastewater samples, octyldimethyl-p-aminobenzoic acid and methylparaben showed the lowest recoveries (20% and 27%). The method revealed benzophenone-3 as having the highest concentration levels ( 7 ng/L) in river waters. Most of PCPs determined were found in influent waters being methylparaben and propylparaben the ones found at highest concentration with values of 5613 and 1945 ng/L, respectively. In effluent waters, significant lower levels of some PCPs were found, being benzophenone-3 the one found at the highest concentration (100 ng/L).
The occurrence, fate, and effects of phenols with endocrine-disrupting properties as well as some pharmaceuticals and personal-care products in the environment have frequently been discussed in recent literature. In many cases, these compounds were determined by using individual methods which can be time-consuming if results for multiple parameters are required. Using a solid-phase extraction procedure with an anion exchanger in this work, we have developed and optimized a multi-residue method for the extraction of 21 phenols and acids in sewage influent and effluent. The phenols and acids were then selectively eluted in separate fractions and were converted into pentafluoropropionyl (PFP) and tert-butyldimethylsilyl (TBDMS) derivatives, respectively, for gas chromatography-mass spectrometric (GC/MS) determination. When applied to the sewage samples under study, the results for nonylphenol, bisphenol A (BPA), triclosan (TCS), 17ss-estradiol (E2), estrone (E1), salicylic acid, ibuprofen, naproxen, diclofenac, and a few other acidic drugs were consistent with those determined previously by individual methods. Using the same procedure, we also report, for the first time, the occurrence of 2-phenylphenol and parabens in those sewage samples.
A method has been developed for the determination of 24 household high production volume (HPV) chemicals in municipal wastewater systems using solid-phase extraction (SPE) and analyses using both gas chromatography and liquid chromatography, each with tandem mass spectrometry (GC-MS/MS and LC-MS/MS). Target compounds include pesticides, antioxidants, fragrances, plasticizers, preservatives and personal care products. Method reporting limits ranged from 0.1 to 100 ng/L in water and recoveries for most compounds were between 54 and 112%. Household HPVs were consistently detected in raw sewage entering three full-scale wastewater treatment plants. Compounds such as vanillin, DEET, benzophenone, 3-indolebutyric acid, bisphenol A, triclosan and triclocarban were detected in all wastewater influent and effluent samples, but were significantly lower in the effluent. Many of the remaining compounds were detected in the influent, but below detection in effluent samples. Menthol and phenoxyethanol had the highest observed concentrations in influent samples ranging from 1.5 to 13 microg/L for menthol, and 8.8 to 22 microg/L for phenoxyethanol. MGK-11, methylresorcinol, trifluralin, hexabromododecane, acriflavin and atrazine were not detected in any samples. The method described here detects a broad range of HPV chemicals with great sensitivity and selectivity.
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