Determination of steroid estrogens in wastewater by high performance liquid chromatography–tandem mass spectrometry

Koh, Y.K.K.; Chiu, T.Y.; Boobis, Alan R.; Cartmell, Elise; Lester, J.N.; Scrimshaw, Mark D.

doi:10.1016/j.chroma.2007.09.074

Cited by 102 publications

(60 citation statements)

References 48 publications

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“…Free estrogen concentrations were consistent with other wastewater effluents (Gentili, Perret et al 2002;D'Ascenzo, Di Corcia et al 2003;Lagana, Bacaloni et al 2004;Zuehlke, Duennbier et al 2005;Lien, Chen et al 2009), but we found generally lower concentrations of sulfate conjugates than expected based on previous studies (Koh, Chiu et al 2007;). In contrast, halogenated forms, especially monoBrE2 and diClE2, were present at unexpectedly high concentrations -on par with, or greater than, free forms.…”

Section: Estrogen Concentration and Potency In Treated Wastewater Effsupporting

confidence: 92%

Natural and synthetic estrogens in wastewater treatment plant effluent and the coastal ocean

Griffith¹

2013

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Steroidal estrogens are potent endocrine disrupting chemicals that are naturally excreted by vertebrates (e.g., humans and fish) and can enter natural waters through the discharge of treated and raw sewage. Because estrogens are detrimental to aquatic organisms at picomolar concentrations, many studies have measured so-called "free" estrogen concentrations in wastewater effluents, rivers, and lakes. Yet, to our knowledge, no studies have characterized the broader range of estrogens that includes free, conjugated, and halogenated forms.Conjugated estrogens are important because they can be easily converted to potent free forms by bacteria in wastewater treatment plants and receiving waters. And halogenated estrogens, produced during wastewater disinfection, are only slightly less potent than free estrogens but much more likely to bioaccumulate.We have developed a tandem mass spectrometry method that is capable of simultaneously quantifying free, conjugated, and halogenated estrogens at picomolar levels in wastewater effluent and coastal seawater. The method was validated using treated effluent from the greater Boston metropolitan area, where we found that halogenated estrogens represented over 50 % of the total estrogen discharge flux. A kinetic model of estrogen halogenation was used to predict the distribution of free and halogenated forms in wastewater effluent and suggested that chlorinated estrogens may be formed en route to the wastewater treatment plant.In the receiving waters of Massachusetts Bay, we detected a range of conjugated, free, and halogenated forms at concentrations that were well-predicted by dilution near the sewage outfall. Farther downstream, we found significantly higher estrone concentrations which points to large inputs of estrogens from sources other than sewage. 4Finally, we have used compound-specific measurements of 13 C and 14 C in commercial and pharmaceutical estrogen preparations to evaluate the potential for using carbon isotopes to distinguish between synthetic and endogenous steroids in wastewater and other environmental matrices. Our results show that synthetic estrogens and progestogens exhibit significantly depleted δ 13 C values (~ -30 ‰) compared to endogenous steroids (-16 ‰ to -26 ‰). This isotopic difference should make it possible to apportion synthetic and endogenous hormone sources in complex environments.

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Section: Estrogen Concentration and Potency In Treated Wastewater Effsupporting

confidence: 92%

Natural and synthetic estrogens in wastewater treatment plant effluent and the coastal ocean

Griffith¹

2013

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“…Prominent among these compounds are naturally occurring 17␤-estradiol (E 2 ), estrone (E 1 ), estriol (E 3 ) and synthetic diethylstilbestrol (DES), ethinylestradiol (EE 2 ). Widespread evidences showed that these estrogens with highest estrogenic activity can exhibit adverse effect on reproductive processes in wildlife and humans at low-ng/L concentration [1][2][3][4][5]. Furthermore, new findings indicated that some of these estrogens or their metabolites play a role in human carcinogenesis, such as breast, prostate and ovarian cancer [6][7][8][9], which has become another hotspot these years about the specific biological effect and potential threat for human bodies.…”

Section: Introductionmentioning

confidence: 99%

Determination of estrogens and bisphenol A in bovine milk by automated on-line C30 solid-phase extraction coupled with high-performance liquid chromatography–mass spectrometry

Yan

Zhao

et al. 2009

Journal of Chromatography A

107

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a b s t r a c tUsing triacontyl bonded silica (C 30 ) as on-line solid-phase extraction (SPE) material and a specially designed on-line analytical system which allowed large sample volume injection, a high speed and robust on-line SPE-HPLC-MS method was established for the analysis of five estrogens and bisphenol A (BPA) in milk samples. The milk sample is pretreated with acetonitrile for protein precipitation and then treated with primary secondary amine for the removal of polar impurities in the matrix. Then the pretreated sample can be automatically loaded by a LC pump. For effective extraction, an offshoot with NH 4 Ac solution of high-flow rate was employed to dilute the loaded sample by a mixing tee before sample was loaded onto the C 30 extraction column. In this way, large volume injection (1 mL in this experiment) could be achieved. Some important parameters such as sample loading flow rate, sample dilution ratio and injection volume were optimized. Under the optimized conditions, the recoveries for all analytes range from 71.4 to 97.1% and reproducibility represented as RSDs are less than 15.0% (n = 5) with milk samples spiked at 0.6 and 15 ng/mL of each analyte. To the authors' knowledge, it constitutes the first work describing a C 30 on-line SPE-LC-MS analytical method for the screen and monitoring of these estrogens and BPA in milk.

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“…Domestic and industrial effluents are the most significant input of these substances in the aquatic environment and these compounds and their metabolites are constantly excreted into the sewers environment and continue to accumulate in the environment. The large variety of compounds with effective or potential endocrine disruptor activity, the diversity of environmental matrices where they can occur, their physical and chemical properties (high to moderate polarity) and the usually low concentrations require an accurate and efficient monitoring of these endocrine disruptors in water sources and water for human consumption Liquid-chromatography coupled to tandem mass spectrometry (LC-MS/MS) is being applied with success to the analysis of these compounds [21][22][23][24][25][26].…”

Section: Introductionmentioning

confidence: 99%

Simultaneous Determination of Ten Endocrine Hormone Disrupters in Water Using SPE/LC-(ESI)MS-MS

Henriques¹,

Cardoso²,

Rodrigues³

et al. 2010

JWARP

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The aim of this study was developed and validated an analytical method based on liquid chromatography and tandem mass spectrometry after solid phase extraction to monitorizing ten endocrine hormone disrupters in Lisbon drinking water system. Natural and synthetic hormones (17-β-estradiol, ethinylestradiol, estriol, estrone, progesterone, mestranol and diethylstilbestrol) and some industrial products (4-n-nonylphenol, 4-tert-octylphenol and bisphenol A) were studied. Mass spectrometer detection parameters were optimized, such as the best conditions for the precursor ion formation, namely cone voltage, when applying negative and positive electrospray ionization, and also collision energy for MRM1 and MRM2 transitions. The best conditions of the solid phase extraction (SPE) using Waters Oasis HLB (6 mL, 200 mg) and Isolute C18 (EC) (6 ml, 1000 mg) were also optimized. The method was validated through the application of several statistical tests and the uncertainty estimation of the analytical assay. This method showed a very good linear range for all the studied analytes with determination coefficients (r 2 ) between 0.9962 and 0.9999 and coefficients of variation lower than 4%. There were no significant differences between recoveries obtained with the studied matrices, like groundwater, surface water and water for human consumption. In these matrices, the recovery values varied between 32 and 95%. The limits of method detection were between 0.28 and 22 ng/L. The validated method was applied for the analysis of water samples from the EPAL (Empresa Portuguesa das Águas Livres, S.A.) water supply system including tap water, spring water, groundwater, and river water. Some target compounds (bisphenol A, progesterone, 4-tert-octylphenol, and 4-n-nonylphenol) were found in trace amounts in analysed waters.

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Determination of steroid estrogens in wastewater by high performance liquid chromatography–tandem mass spectrometry

Cited by 102 publications

References 48 publications

Natural and synthetic estrogens in wastewater treatment plant effluent and the coastal ocean

Natural and synthetic estrogens in wastewater treatment plant effluent and the coastal ocean

Determination of estrogens and bisphenol A in bovine milk by automated on-line C30 solid-phase extraction coupled with high-performance liquid chromatography–mass spectrometry

Simultaneous Determination of Ten Endocrine Hormone Disrupters in Water Using SPE/LC-(ESI)MS-MS

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