Determination of 17β-estradiol and 17α-ethinylestradiol in water at sub-ppt levels by liquid chromatography coupled to tandem mass spectrometry

Ripollés, Cristina; Ibáñez, María; Sancho, Juan V.; López, Francisco J.; Hernández, Félix

doi:10.1039/c4ay00479e

Cited by 28 publications

(14 citation statements)

References 42 publications

(63 reference statements)

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“…EE2 could be detected over 1nG/L with a 50% chance (Aris et al 2014). No detectable amount of E2 and EE2 were found in surface waters at the Mediterranean Spanish coast (with LOD 0.06 and 0.02 ng/L, respectively) (Ripolles et al 2014). Neither E2 nor EE2 could be found in River Tiber and River Aniene (Italy, LODs: 10ng/L) (Patrolecco et al 2015).…”

Section: Discussionmentioning

confidence: 93%

“…These limits are 0.035 ng/L for EE2 and 0.4 ng/L for E2 (European Parliament 2015). These contaminants in an average equipped laboratory using multiresidue analysis without derivatization can only be determined with poor LOQ values (Liu et al 2011b, Loos et al 2010, Ripolles et al 2014). Our methodology with dansyl derivatization is cheap, quick and simple enough to be considered for use in monitoring studies in the future.…”

Section: Discussionmentioning

confidence: 99%

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β-Estradiol and ethinyl-estradiol contamination in the rivers of the Carpathian Basin

Avar

Zrínyi²,

Maász

et al. 2016

Environ Sci Pollut Res

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17β-estradiol (E2) and 17α-ethinyl estradiol (EE2), which are environmental estrogens have been determined with LC-MS in freshwater. Their sensitive analysis needs derivatisation and therefore is very hard to achieve in multiresidue screening. We analysed samples from all the large and some small rivers (River Danube, Drava, Mur, Sava, Tisza and Zala) of the Carpathian Basin and from Lake Balaton. Freshwater was extracted on solid phase and derivatised using dansyl-chloride. Separation was performed on a Kinetex XB-C18 column. Detection was achieved with a benchtop orbitrap mass spectrometer using targeted MS analysis for quantification. Limits of quantification were 0.05 ng/L (MS1) and 0.1 ng/L (MS/MS) for E2, and 0.001 ng/L (MS1) and 0.2 ng/L (MS/MS) for EE2. River samples contained n.d.-5.2 ng/L E2 and n.d.-0.68 ng/L EE2. Average levels of E2 and EE2 were 0.61 and 0.084 ng/L respectively in rivers, water courses and Lake Balaton together, but not counting city canal water. EE2 was less abundant, but it was still present in almost all of the samples. In beach water samples from Lake Balaton we measured 0.076-0.233 E2 and n.d.-0.133 EE2. A relative high amount of EE2 was found in river Zala (0.68 ng/L) and in Hévíz-Páhoki canal (0.52 ng/L), which are both in the catchment area of Lake Balaton (Hungary). HighlightsMethod is proposed for simultaneous determination of 17β-estradiol and 17α-ethinyl estradiol. Derivatization is necessary to reach low LOQ. Low ng/L presence of estrogens in selected European Rivers has been detected.

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Section: Discussionmentioning

confidence: 93%

Section: Discussionmentioning

confidence: 99%

β-Estradiol and ethinyl-estradiol contamination in the rivers of the Carpathian Basin

Avar

Zrínyi²,

Maász

et al. 2016

Environ Sci Pollut Res

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“…The main challenge in the determination of estrogens in wastewater samples is the development of sensitive extraction and preconcentration methodologies that allow the quantification of this type of compound, which are usually found at very low concentrations. SPE is widely used as a routine technique for the determination of EDCs in environmental water samples . Nevertheless, with complex samples such as wastewater influents, the extraction efficiency should be lower than for cleaner samples due to the interferences that are retained in the cartridge .…”

Section: Introductionmentioning

confidence: 99%

Molecularly imprinted solid-phase extraction coupled with ultra high performance liquid chromatography and fluorescence detection for the determination of estrogens and their metabolites in wastewater

et al. 2015

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Estrogens are an important class of endocrine-disrupting compounds, and their contamination of environmental waters through the effluents of wastewater treatment plants could have an important impact on aquatic biota, even at low concentrations. For this reason, the development of selective and sensitive extraction methodologies, which permit the identification and quantification of these compounds at trace level concentrations, is very important. In this study, a quantitative method based on molecularly imprinted solid phase extraction coupled to ultra high performance liquid chromatography with fluorescence detection has been developed. It has been used for the simultaneous determination of three estrogens and two of their metabolites in water samples from wastewater treatment plants. The method developed presents satisfactory limits of detection (between 0.18 and 0.45 ng·mL ), good recoveries (higher than 60%) and low relative standard deviations (under 10%). The method was used to analyze wastewater from a veterinary hospital as well as influent and effluent samples of a wastewater treatment plant of Gran Canaria (Spain) The concentrations of the detected hormones ranged from 1.35 to 2.57 ng·mL .

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“…5 It remains among the most widely used techniques and many publications can be found in the recent literature which utilize mass spectrometric determination of estrogens. 40,43 Methods using liquid chromatography with UV and fluorescence detections are also reported in recent literature. 40,43 Methods using liquid chromatography with UV and fluorescence detections are also reported in recent literature.…”

Section: Recent Advancements In Detection Methodsmentioning

confidence: 99%

“…16,22,[24][25] Fluorescence is a highly sensitive detection method, and yet it suffers from matrix interferences when it comes to complicated environmental samples. [40][41][42][43] Even though MS is a well-established detection method, it still provides room for innovation. 12,17 Hyphenated tandem mass spectrometric determination is considered as the most popular MS method for the determination of estrogens in environmental and food samples.…”

Section: Chromatographic and Hyphenated Mass Spectrometric Methodsmentioning

confidence: 99%

Recent advancements in analytical methods for the determination of steroidal estrogen residues in environmental and food matrices

Gunatilake¹,

Munasinghe²,

Ranaweera³

et al. 2016

Anal. Methods

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Residue steroidal estrogens in environmental and food samples have become a cause for concern as they can affect organisms at low ppt concentrations. Analytical method development plays a key role in trace estrogen analysis due to the combination of low concentrations and complicated sample matrices. Reliable quantification of these trace level steroidal estrogens has become a major concern during the past decade. This mini review focuses on advancements in analytical methods developed for estrogen detection and quantification in environmental and food samples from 2014 -2016. A comprehensive overview of the novelties and the advantages of the recently developed sample pre-concentration, clean-up, and detection methods are discussed. During the past three years, a wide variety of sample extraction methods including, the utilization of innovative imprinted magnetic sorbents, QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and various microextraction methods such as Dispersive liquid-liquid micro extraction (DLLME), Thin film micro extraction (TFME), Solid phase microextraction (SPME), and Vortex assisted hollow fiber liquid-phase micro extraction (VA-HF-LPME) have been

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Determination of 17β-estradiol and 17α-ethinylestradiol in water at sub-ppt levels by liquid chromatography coupled to tandem mass spectrometry

Cited by 28 publications

References 42 publications

β-Estradiol and ethinyl-estradiol contamination in the rivers of the Carpathian Basin

β-Estradiol and ethinyl-estradiol contamination in the rivers of the Carpathian Basin

Molecularly imprinted solid-phase extraction coupled with ultra high performance liquid chromatography and fluorescence detection for the determination of estrogens and their metabolites in wastewater

Recent advancements in analytical methods for the determination of steroidal estrogen residues in environmental and food matrices

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