A method consisting of solid-phase isotope dansylation (derivatization with dansyl chloride) and liquid chromatography-high resolution mass spectrometry (LC-HRMS) was developed for the quantitative analysis of phenolic compounds (phenols) in environmental samples. A magnetic-HLB (hydrophilic lipophilic balanced) material was synthesized and applied as an adsorbent in magnetic solid-phase extraction (MSPE) for the enrichment of the analytical targets. Furthermore, with the solid-phase isotope labeling, the desalting and removal of labeling residuals could be simplified over conventional in-solution labeling. In addition to overcoming the matrix effect by isotope dansylation, the sensitivity for the analysis of phenols by LC-HRMS was remarkably improved by over 100-fold. The method was systematically verified, and good accuracy (86.5–104.9%) and precision (<8.6% and <11.4% for intra- and inter-day, respectively) were achieved for the tested 15 phenols. The limits of detection (LODs) of this method were estimated to be 0.2–5 ng L−1 and 5–100 ng kg−1 in estuary water and sediment samples, respectively. With this method, samples collected from the Daliao River estuary (Panjin, China) were analyzed. It was found that all of the targeted phenols were detected at concentrations ranging from unquantifiable to 485 ng L−1 (the total concentration of analytes found in each sample were in the range 822–957 ng L−1) and unquantifiable to 1368 ng kg−1 (the total concentration of analytes found in each sample were in the range 2251–2992 ng kg−1) in water and sediment, respectively.
Estrogens distribute widely in the environment as endocrine-disrupting chemicals (EDCs), which have to be monitored to evaluate their environmental impact. Aim to improve the analytical throughput of liquid chromatography-high resolution mass spectrometry (LC-HRMS), a quadruplex stable isotope dansylation method was developed, with which three real samples could be quantitatively analyzed in one injection. As the estrogens were at trace level in complex matrices, magnetic solid-phase extraction (MSPE) was applied to enrich these analytes and remove the interfaces. By integrating MSPE and quadruplex stable isotope dansylation, a solid-phase quadruplex labeling method was developed for the LC-HRMS analysis of estrogen analogues . For the tested seven estrogens, the developed method showed low detection limits (0.1–0.5 ng/L for pond water and 0.01–0.05 μg/kg for poultry manure), good precision (RSD < 5.5%) and accuracy (96.8–108.3%). The method was applied in the determination of estrogens in environmental samples, and the results revealed that all the tested estrogens were present in the estuary water (unquantifiable to 71.2 ng/L) and chicken manure (undetectable to 25.43 μg/kg).
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