An analytical method for the simultaneous trace determination of acidic pharmaceuticals and phenolic endocrine disrupting chemicals in wastewater and sewage sludge by gas chromatography-mass spectrometry

摘要: This article presents an analytical method based on solid-phase extraction (SPE) and gas chromatography coupled with mass spectrometry for the simultaneous determination of most frequently used acidic pharmaceutical residues, ibuprofen, diclofenac, naproxen ketoprofen (KFN), phenolic endocrine disruptors, bisphenol (BPA), triclosan (TCS), nonylphenol, nonylphenol monoethoxylate diethoxylate, in wastewater sewage sludge samples. In first phase study, each compound has been characterized individually afterwards mixture as a trimethylsilyl derivative order to identify characteristic ions (m/z ratio) constituting spectrum choose quantification confirmation. Subsequently, derivatization was evaluated by testing different variables such volume solvent bis(trimethylsilyl)trifluoroacetamide effect catalyst, pyridine 1% trimethyl chlorosilane, derivatized solution. For analysis samples, two commercial SPE cartridges, C18 Oasis HLB, were compared their efficiency target compounds. The key parameter procedure included pH (2.5, 5.3 7) loading solid parameters extracted biomass, organic matrix interferences chromatographic evaluated. By using cartridges purification ultrasound sonication, satisfactory mean relative recoveries BPA-d16 meclofenamic acid surrogates obtained ranging from 91% 117% 84% 107% Nine-point calibration standard performed linear regression correlation coefficient >0.99 all tested Limits detection developed methods established between 0.3 (KFN) 14.8 (BPA) ng L−1, 15.0 (TCS) 32.9 g−1 sludge, respectively. Application real samples treatment plant Athens, capital Greece, demonstrated presence compounds