Development of a separation framework for effects-based targeted and non-targeted toxicological screening of water and wastewater

Factors Affecting Sampling Strategies for Design of an Effects‐Directed Analysis for Endocrine‐Active Chemicals

“…For example, relative potency values (or any evidence of estrogenic activity) for identified alkylphenols in an EDA study had not been established in the bioassay, and therefore that study was listed in Table 1 as identifying no active EACs (Thomas et al 2004). Conversely, another EDA study of wastewater was able to identify and quantify 3 estrogenic compounds (benzophenone and 2 phthalates) via nontargeted analysis and establish relative potency values in the bioassay utilized in the EDA, thus allowing CEQ calculations for the active fractions (Pochiraju et al 2020). Although the remainder of the EDA studies in Table 1 were able to identify "active" chemicals in the whole extract and/or fractions, many of those studies did not link the identified EACs to activity in whole extract (that is, did not obtain CEQ to BEQ ratios for both the whole extract and the fractions).…”

“…Not only can EDA guide the identification of the responsible EACs, but it can also help rule out candidate EACs not responsible for the observed biological activity or effect(s). The technique can be necessary when cytotoxic or interfering chemicals in the whole sample prevent accurate assessment of bioactivity (Hashmi et al 2020;Pochiraju et al 2020). This is accomplished through fractionation of the sample extract, using a bioassay to target "active" fractions (i.e., fractions that induce activity in a particular bioassay) for further subfractionation until the resulting active fractions are sufficiently clean to allow identification of the active components (Zwart et al 2018;Hashmi et al 2020).…”

“…In addition, EDA is sometimes not possible due to the low concentrations of EACs often found in environmental waters (analytical chemistry detector limitations), and/or bioassay detection limitations. Flow diagrams for EDA exist in the literature that follow a common pattern of sample collection, extraction, crude fractionation, and fine fractionation (with bioassay assessment of extracts/fractions at each step; Reineke et al 2002;Furuichi et al 2004;Brennan et al 2013;Fetter et al 2014;Pochiraju et al 2020). Using these flow diagrams as a framework, a conceptual EDA could provide investigators with a quick, inexpensive assessment of the elements required to successfully implement an EDA.…”

Molecular Characterization of Estrogen Receptor Agonists during Sewage Treatment Processes Using Effect-Directed Analysis Combined with High-Resolution Full-Scan Screening

“…In parallel, the development of library-matching software makes it easy to search for information on the identification, appearance, and relevance of candidate compounds based on the molecular mass by matching compounds with chromatograms from the instrumental analysis . Previous studies successfully identified unmonitored toxicants in environmental samples using FSA. , For example, ER agonists have been identified in wastewater, including benzophenone, diethyl phthalate, and diisobutyl phthalate …”

“…21 Previous studies successfully identified unmonitored toxicants in environmental samples using FSA. 10,22 For example, ER agonists have been identified in wastewater, including benzophenone, diethyl phthalate, and diisobutyl phthalate. 22 Fourier transform ion cyclotron resonance MS (FT-ICRMS) is a powerful technique that has a high resolution and high mass accuracy.…”