PMID- 34749185 OWN - NLM STAT- MEDLINE DCOM- 20211130 LR - 20211130 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1659 DP - 2021 Dec 6 TI - Nitrogen-rich carbon nitride as solid-phase microextraction fiber coating for high-efficient pretreatment of polychlorinated biphenyls from environmental samples. PG - 462655 LID - S0021-9673(21)00777-9 [pii] LID - 10.1016/j.chroma.2021.462655 [doi] AB - A two-dimensional nitrogen-rich carbon nitrogen (C(3)N(5)) material was prepared via a facile high temperature thermal polymerization. For the first time, the C(3)N(5) was used as fiber coating of solid-phase microextraction (SPME) to extract and preconcentrate polychlorinated biphenyls (PCBs) before gas chromatography (GC) analysis. The X-ray diffraction, N(2) adsorption-desorption, Fourier transform-infrared spectroscopy, thermogravimetric analysis, and X-ray photoelectron spectroscopy were performed to investigate structure, functional groups, thermal stability, bonding type, element composition, and atomic ratio of C(3)N(5). The two-dimensional planar stacking structure was further verified by scanning electron microscopy and transmission electron microscopy. Five PCBs including PCB-4, PCB-12, PCB-29, PCB-52 and PCB-101 were selected as targets to evaluate performance of SPME fiber. Under the optimal conditions, the method showed a good linear range from 0.01 to 1000 ng/mL with the correlation coefficients (R(2)) higher than 0.9990. Enrichment factors of the method were obtained from 2045 to 3080. The limits of detection (LODs, S/N = 3) and limits of quantification (LOQs, S/N = 10) were calculated as 0.0031-0.0111 ng/mL and 0.01-0.05 ng/mL, respectively. The precisions of intra-day and inter-day were obtained with the relative standard deviations (RSDs) at 1.5-6.6% and 0.8-6.9%, respectively. The fiber-to-fiber producibility was achieved with RSDs ranged from 3.5% to 11.4%. The method was applied to detect PCBs in river water and soil samples. The contents were calculated at 0.040-0.147 ng/mL in water and 0.520-3.218 ng/g in soil. The C(3)N(5) as SPME fiber coating material may be applied to extract and preconcentrate other environmental pollutants which have similar chemical structures with PCBs. CI - Copyright (c) 2021 Elsevier B.V. All rights reserved. FAU - Zhang, Xiaowan AU - Zhang X AD - Henan International Joint Laboratory of Medicinal Plants Utilization, School of Chemistry and Chemical Engineering, Henan University, Kaifeng 475004, Henan, China. FAU - Han, Lizhen AU - Han L AD - Henan International Joint Laboratory of Medicinal Plants Utilization, School of Chemistry and Chemical Engineering, Henan University, Kaifeng 475004, Henan, China. FAU - Li, Mengyuan AU - Li M AD - Henan International Joint Laboratory of Medicinal Plants Utilization, School of Chemistry and Chemical Engineering, Henan University, Kaifeng 475004, Henan, China. FAU - Qin, Peige AU - Qin P AD - Henan International Joint Laboratory of Medicinal Plants Utilization, School of Chemistry and Chemical Engineering, Henan University, Kaifeng 475004, Henan, China. FAU - Li, Dan AU - Li D AD - Henan International Joint Laboratory of Medicinal Plants Utilization, School of Chemistry and Chemical Engineering, Henan University, Kaifeng 475004, Henan, China. FAU - Zhou, Qian AU - Zhou Q AD - Henan International Joint Laboratory of Medicinal Plants Utilization, School of Chemistry and Chemical Engineering, Henan University, Kaifeng 475004, Henan, China. FAU - Lu, Minghua AU - Lu M AD - Henan International Joint Laboratory of Medicinal Plants Utilization, School of Chemistry and Chemical Engineering, Henan University, Kaifeng 475004, Henan, China. Electronic address: mhlu@henu.edu.cn. FAU - Cai, Zongwei AU - Cai Z AD - State Key Laboratory of Environmental and Biological Analysis, Department of Chemistry, Hong Kong Baptist University, Hong Kong SAR. LA - eng PT - Journal Article DEP - 20211030 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Nitriles) RN - 534Q0F66RK (cyanogen) RN - DFC2HB4I0K (Polychlorinated Biphenyls) RN - N762921K75 (Nitrogen) SB - IM MH - Nitriles MH - Nitrogen MH - *Polychlorinated Biphenyls MH - *Solid Phase Microextraction OTO - NOTNLM OT - Carbon nitride OT - Environment pollutants OT - Polychlorinated biphenyls OT - Preconcentration OT - Sample pretreatment OT - Solid-phase microextraction COIS- Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. EDAT- 2021/11/09 06:00 MHDA- 2021/12/01 06:00 CRDT- 2021/11/08 20:25 PHST- 2021/05/24 00:00 [received] PHST- 2021/10/21 00:00 [revised] PHST- 2021/10/27 00:00 [accepted] PHST- 2021/11/09 06:00 [pubmed] PHST- 2021/12/01 06:00 [medline] PHST- 2021/11/08 20:25 [entrez] AID - S0021-9673(21)00777-9 [pii] AID - 10.1016/j.chroma.2021.462655 [doi] PST - ppublish SO - J Chromatogr A. 2021 Dec 6;1659:462655. doi: 10.1016/j.chroma.2021.462655. Epub 2021 Oct 30.