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

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