PMID- 28283719 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20180117 LR - 20180117 IS - 1618-2650 (Electronic) IS - 1618-2642 (Linking) VI - 409 IP - 13 DP - 2017 May TI - Facile preparation of hexadecyl-functionalized magnetic core-shell microsphere for the extraction of polychlorinated biphenyls in environmental waters. PG - 3337-3346 LID - 10.1007/s00216-017-0278-x [doi] AB - Alkyl moieties which can retain target analytes due to their lipophilicity are important in sample preparation. In this work, hexadecyl-functionalized magnetic core-shell microspheres (Fe(3)O(4)@SiO(2)-C(16)) was successfully prepared by one-pot sol-gel method and used for magnetic solid-phase extraction of polychlorinated biphenyls (PCBs) in environmental water samples. Optimized preparation method was achieved by altering the adding moment of hexadecyl-silane. The resultant materials were systematically characterized by scanning electron microscope, transmission electron microscope, Fourier transform infrared spectroscopy, energy dispersive X-ray spectrometry, tensionmeter, and vibrating sample magnetometer. The results demonstrated that the optimized adsorbent exhibited core-shell structure, superparamagnetic (66 emu/g), and extremely hydrophobic (water contact angle of 122 degrees ) properties. To evaluate the extraction performance, the prepared material coupled with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) was applied to determinate PCBs. The extraction conditions were optimized. Under the optimal conditions, the proposed method showed a good linearity range of 1-100 ng L(-1) with correlation coefficients (R) of 0.9989-0.9993. Based on a signal-to-noise ratio of 3 and 10, the limits of detection (LODs) and limits of quantification (LOQs) were in the range 0.14-0.27 and 0.39-0.91 ng L(-1), respectively. The intra- and inter-day relative standard deviations (RSDs) were less than 9.06%. The absolute recoveries of PCBs in spiked real water samples were in the range of 75.17 to 101.20%. Additionally, reusability and batch-to-batch reproducibility of the resultant material were acceptable with RSDs less than 5.64 and 3.25%, respectively. Graphical Abstract The synthesis procedure of Fe(3)O(4)@SiO(2)-C(16) and determination of PCBs in water sample 129 x 50 mm (300 x 300 DPI). FAU - Fan, Yu-Han AU - Fan YH AD - State Key Laboratory of Biogeology and Environmental Geology, China University of Geosciences, Wuhan, Hubei, 430074, China. FAU - Zhang, Shou-Wen AU - Zhang SW AD - State Key Laboratory of Biogeology and Environmental Geology, China University of Geosciences, Wuhan, Hubei, 430074, China. FAU - Qin, Shi-Bin AU - Qin SB AD - School of Environmental Studies, China University of Geosciences, Wuhan, 430074, China. FAU - Li, Xiao-Shui AU - Li XS AD - State Key Laboratory of Biogeology and Environmental Geology, China University of Geosciences, Wuhan, Hubei, 430074, China. xmlxsh@sina.com. FAU - Zhang, Yuan AU - Zhang Y AD - State Key Laboratory of Biogeology and Environmental Geology, China University of Geosciences, Wuhan, Hubei, 430074, China. FAU - Qi, Shi-Hua AU - Qi SH AD - State Key Laboratory of Biogeology and Environmental Geology, China University of Geosciences, Wuhan, Hubei, 430074, China. shihuaqi@cug.edu.cn. LA - eng PT - Journal Article DEP - 20170310 PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 OTO - NOTNLM OT - Gas chromatography-tandem mass spectrometry OT - Hexadecyl OT - Magnetic microsphere OT - Polychlorinated biphenyl OT - Water EDAT- 2017/03/12 06:00 MHDA- 2017/03/12 06:01 CRDT- 2017/03/12 06:00 PHST- 2016/12/14 00:00 [received] PHST- 2017/02/22 00:00 [accepted] PHST- 2017/02/20 00:00 [revised] PHST- 2017/03/12 06:00 [pubmed] PHST- 2017/03/12 06:01 [medline] PHST- 2017/03/12 06:00 [entrez] AID - 10.1007/s00216-017-0278-x [pii] AID - 10.1007/s00216-017-0278-x [doi] PST - ppublish SO - Anal Bioanal Chem. 2017 May;409(13):3337-3346. doi: 10.1007/s00216-017-0278-x. Epub 2017 Mar 10.