Simultaneous measurement of free and conjugated estrogens in surface water using capillary liquid chromatography tandem mass spectrometry

Huang, Fan; Karu, Kersti; Campos, Luiza C.

doi:10.1039/d0an02335c

Cited by 16 publications

(6 citation statements)

References 79 publications

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“…2, it is evident that recoveries obtained using cartridges packed with CC/HNO 3 were comparable to the recoveries gained by commercial cartridges. The performance of the proposed method was also comparable with some previously reported methods (Coelho et al 2020;Li et al 2021;Huang et al 2021), where expensive commercial cartridges were used, indicating the cost-effectiveness of this method.…”

Section: Methods Validationsupporting

confidence: 74%

Solid-phase extraction of estrogen hormones from environmental water samples onto chemically modified carbon cryogel

Prokić¹,

Vukčević

Maletić³

et al. 2022

Preprint

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In this study, pristine and chemically treated carbon cryogel (CC) was employed as a solid-phase extraction (SPE) adsorbent for the isolation and enrichment of estrogens from water samples. A novel, sensitive, selective, and cost-effective analytical method for the determination of estrone, 17β-estradiol, and 17α-ethinylestradiol, based on solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS), was developed and validated. The SPE procedure was optimized by selecting the appropriate adsorbent mass, the sample volume, the sample pH, and the type and volume of elution solvent. The influence of the chemical treatment of carbon cryogel on extraction efficiency was also studied, and it was shown that HNO3 treatment led to a slight increase in recovery values over untreated CC. High recovery values (82–95%) obtained by the optimized extraction method were comparable with the recoveries obtained by commercial cartridges. Finally, the optimized method was successfully applied to the analysis of selected hormones in groundwater, surface water, and wastewater samples. The matrix effect of all tested water types was negligible, indicating the high adsorbent selectivity of examined materials toward observed hormones.

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Section: Methods Validationsupporting

confidence: 74%

Solid-phase extraction of estrogen hormones from environmental water samples onto chemically modified carbon cryogel

Prokić¹,

Vukčević

Maletić³

et al. 2022

Preprint

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“…As seen before, DMIS interacted exclusively with the hydroxyl group on the phenolic ring and it was not reactive with the 17-hydroxyl group of estrogens (represented in Fig. 3 ; Keski-Rahkonen et al, 2015 ; Huang et al, 2021 ). Further, catechol estrogens showed double derivatives, but not mono derivatives as DMIS bound to both hydroxyl groups of the A-ring ( Table 1 ).…”

Section: Resultssupporting

confidence: 59%

Ultrasensitive Quantification of Multiple Estrogens in Songbird Blood and Microdissected Brain by LC-MS/MS

Jalabert

Shock

et al. 2022

eNeuro

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Neuroestrogens are synthesized within the brain and regulate social behavior, learning and memory, and cognition. In song sparrows, Melospiza melodia, 17β-estradiol (17β-E 2 ) promotes aggressive behavior, including during the non-breeding season when circulating steroid levels are low. Estrogens are challenging to measure because they are present at very low levels, and current techniques often lack the sensitivity required.Furthermore, current methods often focus on 17β-E 2 and disregard other estrogens.Here, we developed and validated a method to measure four estrogens (estrone, 17β-E 2 , 17α-estradiol, estriol) simultaneously in microdissected songbird brain, with high specificity, sensitivity, accuracy, and precision. We used liquid chromatography tandem mass spectrometry (LC-MS/MS), and to improve sensitivity, we derivatized estrogens using 1,2-dimethylimidazole-5-sulfonyl-chloride (DMIS). The straightforward protocol improved sensitivity by 10-fold for some analytes. There is substantial regional variation in neuroestrogen levels in brain areas that regulate social behavior in male song sparrows. For example, the auditory area NCM, which has high aromatase levels, has the highest estrone and 17β-E 2 levels. In contrast, estrogen levels in blood are very low. Estrogen levels in both brain and circulation are lower in the non-breeding season than in the breeding season. This technique will be useful for estrogen measurement in songbirds and potentially other animal models.

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“…Sulphate steroid conjugates have low logP and high aqueous solubility values (logS), as seen in Table S1, indicating hydrophilic characteristics leading to their occurrence in water samples. Nevertheless, low concentrations, <10.4 pg•L −1 [55], <LOD [56], and up to 1.46 ng•L −1 in Spain [45], have been reported in surface waters upon dilution once entering the…”

Section: Steroid Hormonesmentioning

confidence: 99%

International Comparison, Risk Assessment, and Prioritisation of 26 Endocrine Disrupting Compounds in Three European River Catchments in the UK, Ireland, and Spain

et al. 2023

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Endocrine-disrupting compounds (EDCs) constitute a wide variety of chemistries with diverse properties that may/can pose risks to both humans and the environment. Herein, a total of 26 compounds, including steroids, flame retardants, and plasticizers, were monitored in three major and heavily urbanized river catchments: the R. Liffey (Ireland), the R. Thames (UK), and the R. Ter (Spain), by using a single solid-phase extraction liquid chromatography-mass spectrometry (SPE-LC-MS/MS) method. Occurrence and frequency rates were investigated across all locations over a 10-week period, with the highest concentration obtained for the flame retardant tris(2-chloroethyl) phosphate (TCEP) at 4767 ng∙L−1 in the R. Thames in Central London. Geographical variations were observed between sites and were partially explained using principal component analysis (PCA) and hierarchical cluster analysis (HCA). In particular, discrimination between the R. Ter and the R. Thames was observed based on the presence and concentration of flame retardants, benzotriazole, and steroids. Environmental risk assessment (ERA) across sites showed that caffeine, a chemical marker, and bisphenol A (BPA), a plasticizer, were classified as high-risk for the R. Liffey and R. Thames, based on relative risk quotients (rRQs), and that caffeine was classified as high-risk for the R. Ter, based on RQs. The total risks at each location, namely ΣRQriver, and ΣrRQriver, were: 361, 455, and 723 for the rivers Liffey, Thames, and Ter, respectively. Caffeine, as expected, was ubiquitous in all 3 urban areas, though with the highest RQ observed in the R. Ter. High contributions of BPA were also observed across the three matrices. Therefore, these two compounds should be prioritized independently of location. This study represents a comprehensive EDC monitoring comparison between different European cities based on a single analytical method, which allowed for a geographically independent ERA prioritization to be performed.

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Simultaneous measurement of free and conjugated estrogens in surface water using capillary liquid chromatography tandem mass spectrometry

Abstract: Given detrimental impacts induced by estrogens at trace level, determination of them is significant but challenging due to their low content in environmental samples and inherent weak ionisation. A modified...

Cited by 16 publications

References 79 publications

Solid-phase extraction of estrogen hormones from environmental water samples onto chemically modified carbon cryogel

Solid-phase extraction of estrogen hormones from environmental water samples onto chemically modified carbon cryogel

Ultrasensitive Quantification of Multiple Estrogens in Songbird Blood and Microdissected Brain by LC-MS/MS

International Comparison, Risk Assessment, and Prioritisation of 26 Endocrine Disrupting Compounds in Three European River Catchments in the UK, Ireland, and Spain

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