Analysis of Estrogenic Hormones in Natural Waters, Wastewater and Sludge. Results from the First International Round Robin Test

Esperanza, M.; Herry, Gaëla; Manciot, F.; Laîné, J.M.

doi:10.2166/wpt.2006.033

Cited by 2 publications

(4 citation statements)

References 6 publications

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“…All steroid FN rates increased in the SW comparison, most likely because the spike levels were lowered for this round and the matrix was more complex. These results agree with previous work that suggests steroidal analysis may be difficult at concentrations ∼5 ng/L, depending on whether single- or triple-quadrupole instruments were used. The elevated false positive and false negative rates of some analytes underscore the susceptibility of samples to blank contamination and/or improper determination of detection/quantification levels for analysis at low ng/L levels.…”

Section: Resultssupporting

confidence: 92%

“…In contrast with previous studies, , no trends or correlations were found between overall bias and experience or extraction technique; however, methods employing LC–MS/MS were able to achieve overall biases of <10% for most compounds (Table ), while GC/MS methods were consistently in the lower 50th percentile. These conclusions agree with a previous interlaboratory comparison study but disagree with two others, , although one of these studies found that GC/MS led to the presence of more outliers . In most cases, a single ionization technique was shared by all methods within a particular instrumental class (e.g., all EI for GC/MS vs all ESI– for LC–MS/MS), with the notable exception being the steroids.…”

Section: Resultssupporting

confidence: 82%

“…Of those, 14 showed a decrease of >15%. As the second comparison was designed to challenge the methods with a higher degree of matrix interferences and lower spike amounts, this was not unexpected and agrees with the literature. − Nevertheless, this demonstrates the increased inaccuracy of methods for these compounds at low ng/L levels.…”

Section: Resultssupporting

confidence: 76%

“…Sengl and Krezmer focused mainly on analgesics and β-blockers with between 11 and 20 laboratories while Farre et al conducted their comparison on nonsteroidal anti-inflammatory drugs and 11–14 laboratories. Another paper investigated three steroids in GW, SW, and WW with between 8 and 12 laboratories . Finally, Drewes et al studied a large group of compounds with three laboratories; however, no study has examined a large number of diverse compounds with a similarly large number of participating laboratories and their methods.…”

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confidence: 99%

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Results of an Interlaboratory Comparison of Analytical Methods for Contaminants of Emerging Concern in Water

et al. 2013

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An evaluation of existing analytical methods used to measure contaminants of emerging concern (CECs) was performed through an interlaboratory comparison involving 25 research and commercial laboratories. In total, 52 methods were used in the single-blind study to determine method accuracy and comparability for 22 target compounds, including pharmaceuticals, personal care products, and steroid hormones, all at ng/L levels in surface and drinking water. Method biases ranged from <10% to well over 100% in both matrixes, suggesting that while some methods are accurate, others can be considerably inaccurate. In addition, the number and degree of outliers identified suggest a high degree of variability may be present between methods currently in use. Three compounds, ciprofloxacin, 4-nonylphenol (NP), and 4-tert-octylphenol (OP), were especially difficult to measure accurately. While most compounds had overall false positive rates of ≤5%, bisphenol A, caffeine, NP, OP, and triclosan had false positive rates >15%. In addition, some methods reported false positives for 17β-estradiol and 17α-ethynylestradiol in unspiked drinking water and deionized water, respectively, at levels higher than published predicted no-effect concentrations for these compounds in the environment. False negative rates were also generally <5%; however, rates were higher for the steroid hormones and some of the more challenging compounds, such as ciprofloxacin. The elevated false positive/negative rates of some analytes emphasize the susceptibility of many current methods to blank contamination, misinterpretation of background interferences, and/or inappropriate setting of detection/quantification levels for analysis at low ng/L levels. The results of both comparisons were collectively assessed to identify parameters that resulted in the best overall method performance. Liquid chromatography-tandem mass spectrometry coupled with the calibration technique of isotope dilution were able to accurately quantify most compounds with an average bias of <10% for both matrixes. These findings suggest that this method of analysis is suitable at environmentally relevant levels for most of the compounds studied. This work underscores the need for robust, standardized analytical methods for CECs to improve data quality, increase comparability between studies, and help reduce false positive and false negative rates.

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Section: Resultssupporting

confidence: 92%

Section: Resultssupporting

confidence: 82%

Section: Resultssupporting

confidence: 76%

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confidence: 99%

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Results of an Interlaboratory Comparison of Analytical Methods for Contaminants of Emerging Concern in Water

et al. 2013

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Reduction of endocrine disruptor emissions in the environment: The benefit of wastewater treatment

et al. 2009

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Exposure assessment of 17α‐ethinylestradiol in surface waters of the United States and Europe

Hannah

D’Aco

Anderson

et al. 2009

Enviro Toxic and Chemistry

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An evaluation of measured and predicted concentrations of 17-ethinylestradiol in surface waters of the United States and Europe was conducted to develop expected long-term exposure concentrations for this compound. Measured environmental concentrations (MECs) in surface waters were identified from the literature. Predicted environmental concentrations (PECs) were generated for European and U.S. watersheds using the GREAT-ER and PhATE models, respectively. The majority of MECs are nondetect and generally consistent with model PECs and conservative mass balance calculations. However, the highest MECs are not consistent with concentrations derived from conservative (worst-case) mass balance estimates or model PECs. A review of analytical methods suggests that tandem or high-resolution mass spectrometry methods with extract cleanup result in lower detection limits and lower reported concentrations consistent with model predictions and bounding estimates. Based on model results using PhATE and GREAT-ER, the 90th-percentile low-flow PECs in surface water are approximately 0.2 and 0.3 ng/L for the United States and Europe, respectively. These levels represent conservative estimates of long-term exposure that can be used for risk assessment purposes. Our analysis also indicates that average concentrations are one to two orders of magnitude lower than these 90th-percentile estimates. Higher reported concentrations (e.g., greater than the 99th-percentile PEC of approximately 1 ng/L) could result from methodological problems or unusual environmental circumstances; however, such concentrations are not representative of levels generally found in the environment, warrant special scrutiny, and are not appropriate for use in risk assessments of long-term exposures.

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Analysis of Estrogenic Hormones in Natural Waters, Wastewater and Sludge. Results from the First International Round Robin Test

Cited by 2 publications

References 6 publications

Results of an Interlaboratory Comparison of Analytical Methods for Contaminants of Emerging Concern in Water

Results of an Interlaboratory Comparison of Analytical Methods for Contaminants of Emerging Concern in Water

Reduction of endocrine disruptor emissions in the environment: The benefit of wastewater treatment

Exposure assessment of 17α‐ethinylestradiol in surface waters of the United States and Europe

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