Method validation for the analysis of estrogens (including conjugated compounds) in aqueous matrices

Miège, Cécile; Bados, Philippe; Brosse, Corinne; Coquery, Marina

doi:10.1016/j.trac.2008.11.005

Cited by 49 publications

(28 citation statements)

References 24 publications

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“…For extraction system selection it is very important to establish the relations/interactions between compounds, sorbent and elution solvents. Thus, the sorbent selection depends basically on the nature matrix and analyte properties, as well as sample loaded, breakthrough volume, recovery and adsorption capacity which are important stage for the analytical method elaboration [6,7,[11][12][13][14][15].…”

Section: Introductionmentioning

confidence: 99%

Polymeric and silica sorbents on endocrine disruptors determination

Vidal

Feitosa

Pessoa

et al. 2014

Desalination and Water Treatment

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A B S T R A C TEndocrine disrupting determination at low concentration levels comprises one of the most important targets in environmental analytical chemistry. In spite of inherent high sensitivities obtained for HPLC, these techniques have some limitations depending on the contaminants. As a result, interest in preconcentration using solid-phase extraction (SPE) still continues increasingly for endocrine disrupting determinations by HPLC due to the high accuracy of this method. In this work, we evaluated three different adsorbents in preconcentration of endocrine disruptors in three different categories: pharmaceuticals (sulphamethoxazole, trimethoprim and diclofenac), hormones (estrone, 17β-estradiolacetate and 17β-estradiol) and plastic materials (bisphenol A) in multicomponent aqueous solution using the combination SPE -HPLC. The adsorbents investigated were such as modified silica (octadecylsilane)-DSC-18 (Supelco) and two polymers, a divinylbenzene-N-vinilpirolidona -Oasis ® HLB (Waters) and a styrene-divinylbenzene modified with butyrolactone-Strata-X™ (Phenomenex). The parameters selected to evaluate the best adsorbent were sample loaded, breakthrough volume, recovery and adsorption capacity. The results showed that the polymeric sorbents Oasis and Strata presented good separation and selective ability, then the most efficient sorbent for the described test was applied to the determination of endocrine disruptor (ED) in a wastewater real sample. Almost all endocrine disruptors studied in the present work were found and quantified in the effluent sample, suggesting the selected cartridge could be useful for preconcentration technique of endocrine disruptors in environmental analytical applications. Correlation analysis identified the adsorption parameters which had the most influence in efficiency of SPE adsorbents, such as initial ED concentration, breakthrough volume and recovery.

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Section: Introductionmentioning

confidence: 99%

Polymeric and silica sorbents on endocrine disruptors determination

Vidal

Feitosa

Pessoa

et al. 2014

Desalination and Water Treatment

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“…A substantial number of LC/MS/MS‐based analytical methods have been reported in the literature for potential endocrine disrupting steroid hormones in environmental samples . Some of these methods achieved trace level detection for selected steroid hormones . However, these prior studies involved either analysis of steroid hormones in multiple experiments using different chromatographic conditions, and/or different ionization modes.…”

Section: Resultsmentioning

confidence: 99%

“…EDCs comprise a wide range of chemicals (including natural and synthetic steroid hormones, pesticides, dioxins, alkylphenols, polychlorinated biphenyls, and furans) which mimic the functions of natural hormones . Among these, perhaps the most potent EDCs belong to the group of natural and synthetic steroid hormones.…”

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confidence: 99%

An ultrahigh‐performance chromatography/tandem mass spectrometry quantitative method for trace analysis of potential endocrine disrupting steroid hormones in estuarine sediments

Mulabagal

Wilson

Hayworth

2017

Rapid Comm Mass Spectrometry

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“…For instance, limits of detection (LOD) and LOQ may be underestimated when determined in standard solutions because matrix effects are not considered. These limits may also be underestimated when evaluated with signal-to-noise (S/N) ratios, as they only represent instrumental limits and repeatability is usually not evaluated [16]. Moreover, trueness and precision of the extraction recoveries are usually determined at a single level of spiking, although they may vary along the concentration range.…”

Section: Validation Of the Optimized Sbse-td-gc-ms/ms Methodsmentioning

confidence: 99%

Use of experimental designs for the optimization of stir bar sorptive extraction coupled to GC–MS/MS and comprehensive validation for the quantification of pesticides in freshwaters

Assoumani¹,

Margoum²,

Guillemain³

et al. 2014

Anal Bioanal Chem

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Although experimental design is a powerful tool, it is rarely used for the development of analytical methods for the determination of organic contaminants in the environment. When investigated factors are interdependent, this methodology allows studying efficiently not only their effects on the response but also the effects of their interactions. A complete and didactic chemometric study is described herein for the optimization of an analytical method involving stir bar sorptive extraction followed by thermal desorption coupled with gas chromatography and tandem mass spectrometry for the rapid quantification of several pesticides in freshwaters. We studied, under controlled conditions, the effects of thermal desorption parameters and the effects of their interactions on the desorption efficiency. The desorption time, temperature, flow, and the injector temperature were optimized through a screening design and a Box-Behnken design. The two sequential designs allowed establishing an optimum set of conditions for maximum response. Then, we present the comprehensive validation and the determination of measurement uncertainty of the optimized method. Limits of quantification determined in different natural waters were in the range of 2.5 to 50 ng L(-1), and recoveries were between 90 and 104 %, depending on the pesticide. The whole method uncertainty, assessed at three concentration levels under intra-laboratory reproducibility conditions, was below 25 % for all tested pesticides. Hence, we optimized and validated a robust analytical method to quantify the target pesticides at low concentration levels in freshwater samples, with a simple, fast, and solventless desorption step.

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Method validation for the analysis of estrogens (including conjugated compounds) in aqueous matrices

Cited by 49 publications

References 24 publications

Polymeric and silica sorbents on endocrine disruptors determination

Polymeric and silica sorbents on endocrine disruptors determination

An ultrahigh‐performance chromatography/tandem mass spectrometry quantitative method for trace analysis of potential endocrine disrupting steroid hormones in estuarine sediments

Use of experimental designs for the optimization of stir bar sorptive extraction coupled to GC–MS/MS and comprehensive validation for the quantification of pesticides in freshwaters

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