Simultaneous Analysis of Multiclass Contaminants of Emerging Concern in Sediments by Liquid Chromatography with Tandem Quadrupole Mass Spectrometry

Abstract

A quick, easy, cheap, effective, rugged, and safe (QuEChERS)‐based extraction and simultaneous dispersive solid‐phase extraction (dSPE) clean‐up method was developed for contaminants of emerging concern (CECs) in sediment samples. Hydration with a phosphate buffer (pH 2.0) and salting out with NaCl and MgSO4 facilitated the extraction and liquid–liquid portioning of the aqueous and organic phases. Cleanup of the extracts was achieved by florisil and C18 (1:1) sorbents in dSPE with minimal compromise of the analytes. The extracts were clean enough for determination by liquid chromatography–tandem mass spectrometry (LC‐MS/MS). The procedure was validated for preservatives, blood lipid regulators, analgesics and anti‐inflammatory drugs, plasticizers, and other classes of CECs in sediment matrix spiked at 6 levels between 1‐ and 40‐fold concentrations for CECs of varying analytical sensitivities. The recovery values were generally between approximately 27 and 120% and the relative standard deviation (%RSD) values were below 20% at 10‐ , 20‐ , and 40‐fold spiking levels, albeit the recoveries for some analytes dropped at low spike concentrations. The method showed high sensitivity where the method detection limits (MDLs) were at low ppb levels for the majority of the analytes that ranged between 0.002 and 1.93 µg/kg. The method performance was also compared with well‐established US Environmental Protection Agency (USEPA) Method 1694 by analyzing sediment samples collected from Yundang Lagoon (Xiamen, China) with field‐incurred CEC residues. The sediment samples were detected with residues of parabens, gemfibrozil, ketoprofen, naproxen, fenoprofen, diclofenac, miconazole, carbamazepine, benzophenon‐3, glibenclamide, sildinafil citrate, and some bisphenol analogues. Environ Toxicol Chem 2019;38:1409–1422. © 2019 SETAC

Contaminants of emerging concern in aquatic environment: Occurrence, monitoring, fate, and risk assessment

“…Residues of gemfibrozil, parabens, ketoprofen, fenoprofen, naproxen, diclofenac, carbamazepine, miconazole, sildenafil citrate, benzophenone-3, glibenclamide, and bisphenol analogues were detected in the sediments sampled from Lagoon Yundang (Xiamen, China) (Rashid, Wang, Li, Yu, & Sun, 2019).…”

“…In recent years, QuEChERS has been considered as one of the novel techniques applied to determine CECs, which comprises both extraction and clean-up steps for complex matrices in environment and provides benefits including shorter time-consuming (quick and easy), less amount of organic solvent use (cheap and safe), high selectivity, and desirable recoveries (rugged). Rashid et al (2019) developed a QuEChERS-based extraction and simultaneous dispersive solid-phase extraction (dSPE) clean-up method for the determination of CECs in sediment. They treated the samples by hydration with phosphate buffer (pH = 2.0) and then salting out with NaCl and MgSO 4 and demonstrated that these procedures facilitated the extraction and the liquid-liquid portioning of the organic and aqueous phases and liquid-liquid portioning, and subsequently made the extracts well prepared for LC-MS/MS determination.…”

“…Rashid et al (2019) developed a QuEChERS‐based extraction and simultaneous dispersive solid‐phase extraction (dSPE) clean‐up method for the determination of CECs in sediment. They treated the samples by hydration with phosphate buffer (pH = 2.0) and then salting out with NaCl and MgSO 4 and demonstrated that these procedures facilitated the extraction and the liquid–liquid portioning of the organic and aqueous phases and liquid–liquid portioning, and subsequently made the extracts well prepared for LC‐MS/MS determination.…”

Reconciliation of Spatiotemporal Influences on Two-Dimensional Distribution and Fate of Emerging Contaminants in a Subtropical River

“…Rivers, being the intermediaries between terrestrial and marine environments, serve as primary sinks for the outcomes of geogenic and anthropogenic activities. They are constantly exposed to a variety of pollutants released directly from the urban communities, via runoff from agricultural farms, or via effluents from wastewater treatment plants. , In this regard, contaminants of emerging concern (CECs) that include pharmaceutical and personal care products (PPCPs) and endocrine-disrupting chemicals (EDCs) are increasingly documented for the real and potential implications on environmental and human health. , CECs may persist in the environment and lead to problems like bioaccumulation, antibiotic resistance, endocrine disruption, and environmental/ecosystem pollution and degradation, which has implications for productivity . In some instances, CECs have been related to water quality attributes of industrial and municipal wastewater, agricultural surface runoff, aquaculture, and more .…”

“…1,2 In this regard, contaminants of emerging concern (CECs) that include pharmaceutical and personal care products (PPCPs) and endocrine-disrupting chemicals (EDCs) are increasingly documented for the real and potential implications on environmental and human health. 3,4 CECs may persist in the environment and lead to problems like bioaccumulation, antibiotic resistance, endocrine disruption, and environmental/ ecosystem pollution and degradation, which has implications for productivity. 5 In some instances, CECs have been related to water quality attributes of industrial and municipal wastewater, agricultural surface runoff, aquaculture, and more.…”