Analysis of Steroid Conjugates in Sewage Influent and Effluent by Liquid Chromatography−Tandem Mass Spectrometry

Reddy, Sharanya; Iden, and Charles R.; Brownawell, Bruce J.

doi:10.1021/ac050699x

Cited by 137 publications

(107 citation statements)

References 33 publications

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“…Isotope dilution for estrogens and androgens will correct for incomplete recovery of non-labeled analogues, and help reduce uncertainty resulting from electrospray ionization variability caused by co-extracted matrix (Ferguson et al, 2001;Reddy et al, 2005). Recovery of target compounds was checked by extraction and analysis of unexposed POCIS sorbent spiked with known amounts of each compound, and averaged between 67% for 11-kT and 132% for E3.…”

Section: Pocis Deployment and Analysis Of Steroid Hormonesmentioning

confidence: 99%

Occurrence and biological effect of exogenous steroids in the Elkhorn River, Nebraska, USA

Kolok

Snow

Kohno

et al. 2007

Science of The Total Environment

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Recent studies of surface waters in North America, Japan, and Europe have reported the presence of steroidogenic agents as contaminants. The current study has three objectives: 1) to determine if steroidogenic compounds are present in the Elkhorn River, 2) to determine if sediments collected from the Elkhorn River can act as a source of steroidogenic compounds to aquatic organisms, and 3) to determine if site-specific biological effects are apparent in the hepatic gene expression of fathead minnows. Evidence was obtained using three approaches: 1) deployment of polar organic chemical integrative samplers (POCIS), 2) deployment of caged fathead minnows, and 3) a laboratory experiment in which POCIS and fish were exposed to sediments from the deployment sites. Deployment sites included: the Elkhorn River immediately downstream from a Nebraska wastewater treatment plant, two waterways (Fisher Creek and Sand Creek) likely to be impacted by runoff from cattle feeding operations, and a reference site unlikely to be impacted by waste water inputs. The PO-CIS extracts were analyzed for a number of natural steroids and metabolites, as well as four different synthetic steroids: ethinylestradiol, zearalonol, 17β-trenbolone and melengestrol acetate. Estrogenic and androgenic metabolites, as well as progesterone and trace levels of melengestrol acetate were detected in POCIS deployed at each site. POCIS deployed in tanks containing field sediments from the four sites did not accumulate the synthetic steroids except for ethinylestradiol, which was detected in the aquarium containing sediments collected near the wastewater treatment plant. Fish deployed in Sand Creek and at the wastewater treatment plant experienced significantly elevated levels of gene expression for two genes (StAR and P450scc) relative to those deployed in Fisher Creek. Fish exposed to the sediments collected from Sand Creek had significantly higher levels of hepatic StAR and P450scc gene expression than did fish exposed to sediments from the two other field sites, as well as the no-sediment control tank. In conclusion: 1) detectable levels of steroidogenic compounds were detected in passive samplers deployed in the Elkhorn River, 2) sediments do not appear to be a significant source for steroidogenic compounds, and 3) site-specific differences were found in mRNA expression among the different treatment groups of fish; however, a functional explanation for these differences is not readily forthcoming.

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Section: Pocis Deployment and Analysis Of Steroid Hormonesmentioning

confidence: 99%

Occurrence and biological effect of exogenous steroids in the Elkhorn River, Nebraska, USA

Kolok

Snow

Kohno

et al. 2007

Science of The Total Environment

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“…Isotope dilution has also been discussed as a means to compensate for matrix effects (14,18,19,21,23,(28)(29)(30). Although is it generally considered the most highly recommended (30) and the most versatile approach (19) for dealing with matrix effects, it has only been used in the past for the analysis of individual compounds or small groups of similar compounds and has been characterized as being costintensive and having a lack of availability (18,24).…”

Section: Introductionmentioning

confidence: 99%

“…Still more have been developed to minimize matrix effects using different extraction, cleanup and elution techniques, including size-exclusion chromatography (18,24), solid-phase extraction (22), LC chromatographic procedures (14,22), ultra performance liquid chromatography (25), hollow fiber liquid-phase microextraction (26), flowsplitting and reduced eluent flow rates (24,27). However, most become problematic when applied to the simultaneous analysis of a broad range of compounds that encompass many different classes and structures in matrices having varying degrees of suppression and enhancement.Isotope dilution has also been discussed as a means to compensate for matrix effects (14,18,19,21,23,(28)(29)(30). Although is it generally considered the most highly recommended (30) and the most versatile approach (19) for dealing with matrix effects, it has only been used in the past for the analysis of individual compounds or small groups of similar compounds and has been characterized as being costintensive and having a lack of availability (18,24).…”

mentioning

confidence: 99%

Analysis of Pharmaceuticals in Water by Isotope Dilution Liquid Chromatography/Tandem Mass Spectrometry

Vanderford

Snyder

2006

Environ. Sci. Technol.

417

222

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A method has been developed for the trace analysis of 15 pharmaceuticals, four metabolites of pharmaceuticals, three potential endocrine disruptors, and one personal care product in various waters. The method employs solidphase extraction (SPE) and liquid chromatography/tandem mass spectrometry (LC-MS/MS), using electrospray ionization (ESI) in both positive and negative modes. Unlike many previous LC-MS/MS methods, which suffer from matrix suppression, this method uses isotope dilution for each compound to correct for matrix suppression, as well as SPE losses and instrument variability. The method was tested in five matrices, and results indicate that the method is very robust. Matrix spike recoveries for all compounds were between 88 and 106% for wastewater influent, 85 and 108% for wastewater effluent, 72 and 105% for surface water impacted by wastewater, 96 and 113% for surface water, and 91 and 116% for drinking water. The method reporting limits for all compounds were between 0.25 and 1.0 ng/L, based on 500 mL of sample extracted and a final extract volume of 500 µL. Occurrence of the compounds in all five matrices is also reported. IntroductionDue to a number of recent reports (1-7), sustained interest in the presence and fate of organic contaminants has been thoroughly established. As concern regarding the environmental impact of exogenous chemicals present in water continues to grow, so too have the number of analytical methods dedicated to their identification and quantification (8,9). This is especially true for the analysis of these compounds by liquid chromatography-mass spectrometry (LC-MS) (10-12). However, even though the number of methods using LC-MS has risen dramatically, discussion of matrix suppression and enhancement that can occur during the use of LC-MS for environmental analysis and the effect it can have on quantification accuracy and precision has been discussed in a relatively small number of publications.Although the cause of matrix effects has been postulated to be natural organic matter (13), the mechanism still has not been fully resolved (14). Regardless, recent reports have shown drastic matrix effects when using LC-MS for the analysis of environmental and biological samples (14-21). There have been a number of methods proposed to compensate for matrix effects by using different calibration techniques, including standard addition (13, 17, 22), surrogate monitoring (15, 20), and various forms of internal calibration (14-16, 19, 23). Still more have been developed to minimize matrix effects using different extraction, cleanup and elution techniques, including size-exclusion chromatography (18,24), solid-phase extraction (22), LC chromatographic procedures (14,22), ultra performance liquid chromatography (25), hollow fiber liquid-phase microextraction (26), flowsplitting and reduced eluent flow rates (24,27). However, most become problematic when applied to the simultaneous analysis of a broad range of compounds that encompass many different classes and structures in matrices havi...

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“…For estrogenic compounds, the metabolites formed are glucuronide and sulfate conjugates and are frequently detected in untreated wastewaters [61]. However, the conjugated estrogens are vulnerable in aerobic activated sludge and end up as free estrogens after de-conjugation [62].…”

Section: Transformation Products (Metabolites) Formed By Human Metabomentioning

confidence: 99%

Targeted and non-targeted liquid chromatography-mass spectrometric workflows for identification of transformation products of emerging pollutants in the aquatic environment

Bletsou

Jeon

Hollender

et al. 2015

TrAC Trends in Analytical Chemistry

295

184

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A B S T R A C TIdentification of transformation products (TPs) of emerging pollutants is challenging, due to the vast number of compounds, mostly unknown, the complexity of the matrices and their often low concentrations, requiring highly selective, highly sensitive techniques. We compile background information on biotic and abiotic formation of TPs and analytical developments over the past five years. We present a database of biotic or abiotic TPs compiled from those identified in recent years. We discuss mass spectrometric (MS) techniques and workflows for target, suspect and non-target screening of TPs with emphasis on liquid chromatography coupled to MS (LC-MS). Both low-and high-resolution (HR) mass analyzers have been applied, but HR-MS is the technique of choice, due to its high confirmatory capabilities, derived from the high resolving power and the mass accuracy in MS and MS/MS modes, and the sophisticated software developed.

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Analysis of Steroid Conjugates in Sewage Influent and Effluent by Liquid Chromatography−Tandem Mass Spectrometry

Cited by 137 publications

References 33 publications

Occurrence and biological effect of exogenous steroids in the Elkhorn River, Nebraska, USA

Occurrence and biological effect of exogenous steroids in the Elkhorn River, Nebraska, USA

Analysis of Pharmaceuticals in Water by Isotope Dilution Liquid Chromatography/Tandem Mass Spectrometry

Targeted and non-targeted liquid chromatography-mass spectrometric workflows for identification of transformation products of emerging pollutants in the aquatic environment

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