Covalent Organic Framework as Fiber Coating for Solid-Phase Microextraction of Chlorophenols Followed by Quantification with Gas Chromatography–Mass Spectrometry

Headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry was adopted for the simultaneous determination of seven chlorophenols (CPs) from honey and canned-yellow-peach samples. A covalent organic framework made of 1,3,5-triformylphloroglucinol (Tp) and benzidine (BD) was used as the SPME fiber coating to preconcentrate the acetylation derivatives of the CPs. The main experimental parameters including derivatization conditions, extraction temperature and time, headspace volume, salt concentration, and desorption temperature were investigated. The fiber showed a high extraction capability for the CPs. The limits of detection (LODs) for the analytes were 0.3–0.7 μg kg–1 for honey and 0.8–1.8 μg kg–1 for canned-yellow-peach samples, suggesting good sensitivity for the method. The response linearity was 2.4–250 μg kg–1 for 2-CP and 3,4-CP and 1.0–150 μg kg–1 for the other remaining analytes in the honey samples. For the canned-yellow-peach samples, the response linearity was 6.0–300 μg kg–1 for 2-CP and 3,4-CP and 3.0–200 μg kg–1 for the others. The correlation coefficients were higher than 0.9919. Good repeatability (RSD < 11.9%) for the method and high recoveries (70.2–113%) of the analytes were observed under the optimal conditions. The established method was satisfactorily applied for the analysis of honey and canned-yellow-peach samples