PMID- 31839356 OWN - NLM STAT- MEDLINE DCOM- 20200526 LR - 20200526 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1615 DP - 2020 Mar 29 TI - In-situ synthesis of fluorinated magnetic covalent organic frameworks for fluorinated magnetic solid-phase extraction of ultratrace perfluorinated compounds from milk. PG - 460773 LID - S0021-9673(19)31221-X [pii] LID - 10.1016/j.chroma.2019.460773 [doi] AB - Perfluorinated compounds (PFCs) are new types of persistent organic pollutants known to bioaccumulate in organism, which have come under increased scrutiny due to the close relation with various health problems. Sensitive detection of PFCs remains a significant challenge because of their ultratrace levels in complex samples. Herein, fluorinated magnetic covalent organic frameworks (Fe(3)O(4)@TpPa-F(4)) were first synthesized via a monomer-mediated in situ growth strategy and served as fluorinated magnetic adsorbent. Accordingly, a novel pretreatment method based on fluorinated magnetic solid-phase extraction (FM-SPE) combined with HPLC-MS/MS was developed to detect ultratrace PFCs from milk samples. The as-prepared Fe(3)O(4)@TpPa-F(4) possessed regular porosity (0.81 nm) with large surface areas (188.04 m(2)/g), high fluorine content (4.85%), strong magnetic responsiveness (50 emu/g), and good chemical and thermal stability, which rendered it an ideal adsorbent material for highly efficient extraction of PFCs. Under the optimized parameters, the developed method displayed good linearity for six PFCs in the range of 0.1-250 ng/L with high correlation coefficients (r >/= 0.9952), and the corresponding limits of detection (LODs) were 0.005-0.05 ng/L (S/N >/= 3). Furthermore, high enrichment factors (EFs, 21.91-100.6 folds) and acceptable relative standard deviations (RSDs) of inter-day (0.5-11.8%) and batch-to-batch (2.3-11.7%) for the six PFCs were achieved. Moreover, this method was further employed to milk samples with different brands and packages, in which ultratrace PFCs were found with diverse concentrations from 10.36 to 729.34 ng/L, confirming the promising applicability of the Fe(3)O(4)@TpPa-F(4) as an alternative adsorbent for sample pretreatment. CI - Copyright (c) 2019 Elsevier B.V. All rights reserved. FAU - Zhang, Mingyue AU - Zhang M AD - Ministry of Education Key Laboratory of Analytical Science for Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian 350116, China. FAU - Li, Jing AU - Li J AD - Ministry of Education Key Laboratory of Analytical Science for Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian 350116, China. FAU - Zhang, Chao AU - Zhang C AD - Ministry of Education Key Laboratory of Analytical Science for Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian 350116, China. FAU - Wu, Zhifeng AU - Wu Z AD - Ministry of Education Key Laboratory of Analytical Science for Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian 350116, China. FAU - Yang, Yixin AU - Yang Y AD - Ministry of Education Key Laboratory of Analytical Science for Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian 350116, China. FAU - Li, Jingguang AU - Li J AD - China National Center for Food Safety Risk Assessment, Beijing 100022, China. FAU - Fu, Fengfu AU - Fu F AD - Ministry of Education Key Laboratory of Analytical Science for Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian 350116, China. Electronic address: fengfu@fzu.edu.cn. FAU - Lin, Zian AU - Lin Z AD - Ministry of Education Key Laboratory of Analytical Science for Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian 350116, China. Electronic address: zianlin@fzu.edu.cn. LA - eng PT - Journal Article DEP - 20191207 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Fluorocarbons) RN - 0 (Metal-Organic Frameworks) RN - 284SYP0193 (Fluorine) SB - IM MH - Animals MH - Chromatography, High Pressure Liquid MH - Fluorine/chemistry MH - Fluorocarbons/*analysis MH - Food Analysis/*methods MH - Limit of Detection MH - Magnetics MH - Metal-Organic Frameworks/*chemical synthesis MH - Milk/*chemistry MH - *Solid Phase Extraction MH - Tandem Mass Spectrometry OTO - NOTNLM OT - Fluorinated magnetic covalent organic frameworks OT - Fluorinated magnetic solid-phase extraction OT - Perfluorinated compounds OT - milk 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. The authors declare the following financial interests/personal relationships which may be considered as potential competing interests. EDAT- 2019/12/17 06:00 MHDA- 2020/05/27 06:00 CRDT- 2019/12/17 06:00 PHST- 2019/11/05 00:00 [received] PHST- 2019/12/06 00:00 [revised] PHST- 2019/12/06 00:00 [accepted] PHST- 2019/12/17 06:00 [pubmed] PHST- 2020/05/27 06:00 [medline] PHST- 2019/12/17 06:00 [entrez] AID - S0021-9673(19)31221-X [pii] AID - 10.1016/j.chroma.2019.460773 [doi] PST - ppublish SO - J Chromatogr A. 2020 Mar 29;1615:460773. doi: 10.1016/j.chroma.2019.460773. Epub 2019 Dec 7.