{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,5,16]],"date-time":"2026-05-16T04:10:35Z","timestamp":1778904635017,"version":"3.51.4"},"reference-count":42,"publisher":"MDPI AG","issue":"21","license":[{"start":{"date-parts":[[2023,11,3]],"date-time":"2023-11-03T00:00:00Z","timestamp":1698969600000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"name":"Science and Technology Program of Zhejiang Province, China","award":["LGC22B050032"],"award-info":[{"award-number":["LGC22B050032"]}]},{"name":"Science and Technology Program of Zhejiang Province, China","award":["LGN22C200018"],"award-info":[{"award-number":["LGN22C200018"]}]},{"name":"Science and Technology Program of Zhejiang Province, China","award":["HYS-CZ-202309"],"award-info":[{"award-number":["HYS-CZ-202309"]}]},{"name":"Special Project of Zhejiang Scientific Research Institute","award":["LGC22B050032"],"award-info":[{"award-number":["LGC22B050032"]}]},{"name":"Special Project of Zhejiang Scientific Research Institute","award":["LGN22C200018"],"award-info":[{"award-number":["LGN22C200018"]}]},{"name":"Special Project of Zhejiang Scientific Research Institute","award":["HYS-CZ-202309"],"award-info":[{"award-number":["HYS-CZ-202309"]}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Molecules"],"abstract":"<jats:p>A magnetic adsorbent based on a C-nanofiber (Fe3O4@C\u2013NFs) nanocomposite was synthesized using a simple one-pot co-precipitation method. The characterized results showed that the obtained C\u2013nanofiber\u2013coated magnetic nanoparticles had many attractive features such as a large specific surface area and a highly interwoven and branched mesoporous structure, as well as distinguished magnetism. The nanocomposite was then used as an adsorbent in the magnetic solid phase extraction (MSPE) of four typical tetracyclines (oxytetracycline, tetracycline, chlortetracycline, and doxycycline) in aquatic products. The TCs in the extract were determined using ultra-high-performance liquid chromatography\u2013tandem mass spectrometry (UHPLC-MS\/MS). Experimental variables of MSPE, including the sorbent amount, pH condition, adsorption and desorption time, and desorption solvent, were investigated and optimized systematically. The method validation indicated that the developed method showed good linearity (R2 &gt; 0.995) in the range of 1.0\u2013200 ng\/mL. The average recoveries at the spiked levels ranged from 90.7% to 102.7% with intra-day and inter-day relative standard deviations (RSDs, n = 6) ranging from 3.72% to 8.17% and 4.20% to 9.69%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for the four kinds of TCs were 0.7 \u03bcg\/kg and 2.0 \u03bcg\/kg, respectively. Finally, MSPE based on C-nanofiber-coated magnetic nanoparticles was successfully applied to TC analysis in real aquatic products (grass carp, large yellow croaker, snakehead, mandarin fish, Penaeus vannamei, swimming crab, etc.). Compared with traditional extraction methods, the proposed method for TC analysis in aquatic products is more sensitive, effective, recyclable, and environmentally friendly.<\/jats:p>","DOI":"10.3390\/molecules28217421","type":"journal-article","created":{"date-parts":[[2023,11,3]],"date-time":"2023-11-03T10:59:54Z","timestamp":1699009194000},"page":"7421","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":10,"title":["One Pot Synthesis of Nanofiber-Coated Magnetic Composites as Magnetic Dispersive Solid-Phase Extraction Adsorbents for Rapid Determination of Tetracyclines in Aquatic Food Products"],"prefix":"10.3390","volume":"28","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-9617-2194","authenticated-orcid":false,"given":"Peipei","family":"Li","sequence":"first","affiliation":[{"name":"Zhejiang Marine Fisheries Research Institute, Tiyu Road 28, Zhoushan 316021, China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Junlu","family":"Bai","sequence":"additional","affiliation":[{"name":"College of Food and Pharmacy, Zhejiang Ocean University, 1 South Haida Road, Zhoushan 316000, China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Pengfei","family":"He","sequence":"additional","affiliation":[{"name":"Zhejiang Marine Fisheries Research Institute, Tiyu Road 28, Zhoushan 316021, China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Junjie","family":"Zeng","sequence":"additional","affiliation":[{"name":"Zhejiang Marine Fisheries Research Institute, Tiyu Road 28, Zhoushan 316021, China"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"1968","published-online":{"date-parts":[[2023,11,3]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"26","DOI":"10.1016\/j.jchromb.2013.02.018","article-title":"Aptamer based extraction followed by electrospray ionization-ion mobility spectrometry for analysis oftetracycline in biological fluids","volume":"925","author":"Aslipashaki","year":"2013","journal-title":"J. Chromatogr. B"},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"424","DOI":"10.1016\/j.foodcont.2015.06.002","article-title":"Development of a novel sensitive molecularly imprinted polymer sensor based on electropolymerization of amicroporous-metal-organic framework for tetracycline detection in honey","volume":"59","author":"Bougrini","year":"2016","journal-title":"Food Control"},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"104170","DOI":"10.1016\/j.microc.2019.104170","article-title":"A simple methodology based on cloud point extraction prior to HPLC-PDA analysis for tetracycline residues in food samples","volume":"150","author":"Saridal","year":"2019","journal-title":"Microchem. J."},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"118196","DOI":"10.1016\/j.molliq.2021.118196","article-title":"Theoretical design and experimental study of new aptamers with the enhanced binding affinity relying on colorimetric assay for tetracycline detection","volume":"349","author":"Nabavi","year":"2022","journal-title":"J. Mol. Liq."},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"21","DOI":"10.3390\/separations6020021","article-title":"Development of a high pressure liquid chromatography with diode array detection method for the determination of four tetracycline residues in milk by using quenchers dispersive extraction","volume":"6","author":"Marinou","year":"2019","journal-title":"Separations"},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"1620","DOI":"10.1007\/s42765-022-00189-w","article-title":"Growth of biobr\/zif-67 nanocomposites on carbon fiber cloth as filter-membrane-shaped photocatalyst for degrading pollutants in flowing wastewater","volume":"4","author":"Li","year":"2022","journal-title":"Adv. Fiber Mater."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"994","DOI":"10.1007\/s42765-022-00253-5","article-title":"Ta3N5\/CdS Core\u2013Shell S-scheme Heterojunction Nanofibers for Efficient Photocatalytic Removal of Antibiotic Tetracycline and Cr(VI): Performance and Mechanism Insights","volume":"5","author":"Li","year":"2023","journal-title":"Adv. Fiber Mater."},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"101","DOI":"10.1016\/S1872-2067(23)64479-1","article-title":"MIL-101(Fe)\/BiOBr S-scheme photocatalyst for promoting photocatalytic abatement of Cr(VI) and enrofloxacin antibiotic: Performance and mechanism","volume":"51","author":"Li","year":"2023","journal-title":"Chin. J. Catal."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"328","DOI":"10.1016\/j.foodchem.2013.11.008","article-title":"Ultrasoundassisted dispersive extraction for the high pressure liquid chromatographic determination of tetracycline residues in milk with diode array detection","volume":"150","author":"Karageorgou","year":"2014","journal-title":"Food Chem."},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"123852","DOI":"10.1016\/j.talanta.2022.123852","article-title":"One-pot co-extraction of dispersive solid phase extraction employing iron-tannic nanoparticles assisted cloud point extraction for the determination of tetracyclines by high-performance liquid chromatography","volume":"252","author":"Phomai","year":"2023","journal-title":"Talanta"},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"111","DOI":"10.1016\/j.chroma.2013.07.084","article-title":"Extraction of tetracyclic antibiotic residues from fish filet: Comparison and optimization of different procedures using liquid chromatography with fluorescence detection","volume":"1307","author":"Orlando","year":"2013","journal-title":"J. Chromatogr. A"},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"53","DOI":"10.1016\/j.chroma.2015.10.035","article-title":"One pot synthesis of magnetic graphene\/carbon nanotube composites as magnetic dispersive solid-phase extraction adsorbent for rapid determination of oxytetracycline in sewage water, Journal of chromatography, A: Including electrophoresis and other separation methods","volume":"1422","author":"Sun","year":"2015","journal-title":"J. Chromatogr. A"},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"1763","DOI":"10.1016\/j.foodchem.2016.10.107","article-title":"Salting-out assisted liquid\u2013liquid extraction coupled to ultra-high performance liquid chromatography\u2013tandem mass spectrometry for the determination of tetracycline residues in infant foods","volume":"221","year":"2017","journal-title":"Food Chem."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"115","DOI":"10.1002\/jssc.201401032","article-title":"Determination of tetracycline antibiotics in fatty food samples by selective pressurized liquid extraction coupled with high performance liquid chromatography and tandem mass spectrometry","volume":"38","author":"Jiao","year":"2014","journal-title":"J. Sep. Sci."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"118","DOI":"10.1016\/j.jfda.2018.06.003","article-title":"Multiclass analysis of antimicrobial drugs in shrimp muscle by ultra high performance liquid chromatography-tandem mass spectrometry","volume":"27","author":"Susakate","year":"2018","journal-title":"J. Food Drug Anal."},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"275","DOI":"10.1016\/j.msec.2014.04.004","article-title":"Magnetic solid-phase extraction based onmesoporous silica-coated magnetic nanoparticles for analysis of oral antidiabetic drugs in human plasma","volume":"40","author":"Andrade","year":"2014","journal-title":"Mater. Sci. Eng. C"},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"26","DOI":"10.1016\/j.trac.2014.03.011","article-title":"Recent advances in solid-phase sorbents for sample preparation prior to chromatographic analysis","volume":"59","author":"Wen","year":"2014","journal-title":"TrAC Trends Anal. Chem."},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"24","DOI":"10.1016\/j.chroma.2017.04.004","article-title":"Towards the determination of sulfonamides in meat samples: Amagnetic and mesoporous metal-organic framework as an efficient sorbent for magnetic solid phase extraction combined with high-performance liquid chromatography","volume":"1500","author":"Xia","year":"2017","journal-title":"J. Chromatogr. A"},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"460543","DOI":"10.1016\/j.chroma.2019.460543","article-title":"Magnetic solid-phase extraction of sulfonamide antibiotics in water and animal-derived food samples using core-shell magnetite and molybdenum disulfide nanocomposite adsorbent","volume":"1610","author":"Zhao","year":"2019","journal-title":"J. Chromatogr. A"},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"2817","DOI":"10.1007\/s00216-019-01726-0","article-title":"Determination of fluoroquinolones in food samples by magnetic solid-phase extraction based on a magnetic molecular sieve nanocomposite prior to high-performance liquid chromatography and tandem mass spectrometry","volume":"411","author":"Yu","year":"2019","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1016\/j.chroma.2017.12.041","article-title":"Magnetic solid\u2013phase extraction of tetracyclines using ferrous oxide coated magnetic silica microspheres from water samples","volume":"1534","author":"Lian","year":"2018","journal-title":"J. Chromatogr. A"},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"238","DOI":"10.1063\/1674-0068\/cjcp2004046","article-title":"Detection of Tetracycline Antibiotics in Water by Dispersive Micro-solid Phase Extraction using Fe3O4@[Cu3(btc)2] Magnetic Composite Combined with Liquid Chromatography-Tandem Mass Spectrometry","volume":"34","author":"Li","year":"2021","journal-title":"Chin. J. Chem. Phys."},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"125952","DOI":"10.1016\/j.cej.2020.125952","article-title":"Adsorption and photocatalytic degradation mechanism of magnetic graphene oxide\/ZnO nanocomposites for tetracycline contaminants","volume":"400","author":"Qiao","year":"2020","journal-title":"Chem. Eng. J."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"2987","DOI":"10.1007\/s11356-016-7964-7","article-title":"Removal of tetracycline and oxytetracycline from water by magnetic Fe3O4@graphene","volume":"24","author":"Zhang","year":"2017","journal-title":"Environ. Sci. Pollut. Res."},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"1601","DOI":"10.1007\/s11696-022-02577-3","article-title":"Preparation, characterization, and application of chitosan-kaolin-based nanocomposite in magnetic solid-phase extraction of tetracycline in aqueous samples","volume":"77","author":"Lefatle","year":"2022","journal-title":"Chem. Pap."},{"key":"ref_26","first-page":"S1570023218307864","article-title":"Determination of three tetracyclines in bovine milk using magnetic solid phase extraction in tandem with dispersive liquid-liquid microextraction coupled with HPLC","volume":"1092","author":"Sereshti","year":"2018","journal-title":"J. Chromatogr. B"},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"122307","DOI":"10.1016\/j.talanta.2021.122307","article-title":"Determination of chloramphenicol and tetracycline residues in milk samples by means of nanofiber coated magnetic particles prior to high-performance liquid chromatography-diode array detection","volume":"230","author":"Vuran","year":"2021","journal-title":"Talanta"},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"1253","DOI":"10.1081\/JLC-200053046","article-title":"UPLC\u2122: An Introduction and Review","volume":"28","author":"Swartz","year":"2005","journal-title":"J. Liq. Chromatogr. Relat. Technol."},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"171","DOI":"10.1016\/j.foodcont.2016.04.050","article-title":"Molecularly imprinted polymer-high performance liquid chromatography for the determination of tetracycline drugs in animal derived foods","volume":"69","author":"Feng","year":"2016","journal-title":"Food Control"},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"1332","DOI":"10.1016\/j.meatsci.2013.11.011","article-title":"Determination of tetracyclines in pig and other meat samples using liquid chromatography coupled with diode array and tandem mass spectrometric detectors","volume":"96","author":"Sharma","year":"2014","journal-title":"Meat Sci."},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"269","DOI":"10.1016\/j.aca.2006.09.025","article-title":"Simultaneous multiresidue determination of tetracyclines and fluoroquinolones in catfish muscle using high performance liquid chromatography with fluorescence detection","volume":"586","author":"Schneider","year":"2007","journal-title":"Anal. Chim. Acta"},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"321","DOI":"10.1016\/j.talanta.2015.11.006","article-title":"Development and application of a dispersive liquid-liquid microextraction method for the determination of tetracyclines in beef by liquid chromatography mass spectrometry","volume":"148","author":"Mookantsa","year":"2016","journal-title":"Talanta"},{"key":"ref_33","doi-asserted-by":"crossref","first-page":"566","DOI":"10.1016\/j.jsps.2021.04.017","article-title":"Determination of tetracycline, oxytetracycline and chlortetracycline residues in seafood products of Saudi Arabia using high performance liquid chromatography\u2014Photo diode array detection","volume":"29","author":"Alanazi","year":"2021","journal-title":"Saudi Pharm. J."},{"key":"ref_34","doi-asserted-by":"crossref","first-page":"252","DOI":"10.1016\/j.foodchem.2016.02.142","article-title":"Multiresidue analysis of sulfonamides, quinolones, and tetracyclines in animal tissues by ultra-high performance liquid chromatography-tandem mass spectrometry","volume":"204","author":"Zhang","year":"2016","journal-title":"Food Chem."},{"key":"ref_35","doi-asserted-by":"crossref","first-page":"2009","DOI":"10.1007\/s00216-009-2641-z","article-title":"Determination of trace tetracycline antibiotics in foodstuffs by liquid chromatography-tandem mass spectrometry coupled with selective molecular-imprinted solid-phase extraction","volume":"393","author":"Jing","year":"2009","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_36","doi-asserted-by":"crossref","first-page":"e217","DOI":"10.1111\/j.1365-2109.2010.02504.x","article-title":"Multiresidue determination of antibiotics in aquaculture fish samples by HPLC\u2013MS\/MS","volume":"41","author":"Maquieira","year":"2010","journal-title":"Aquac. Res."},{"key":"ref_37","doi-asserted-by":"crossref","first-page":"29","DOI":"10.2478\/s11696-013-0428-3","article-title":"Simultaneous determination of 32 antibiotics in aquaculture products using LC-MS\/MS","volume":"68","author":"Fedorova","year":"2014","journal-title":"Chem. Pap."},{"key":"ref_38","doi-asserted-by":"crossref","first-page":"1653","DOI":"10.1080\/00032719.2018.1560458","article-title":"Determination of tetracycline in water and honey by iron(II, III)\/aptamer-based magnetic solid-phase extraction with high-performance liquid chromatography analysis","volume":"52","author":"Tu","year":"2019","journal-title":"Anal. Lett."},{"key":"ref_39","doi-asserted-by":"crossref","first-page":"2884","DOI":"10.1007\/s13197-020-04320-w","article-title":"Development and application of magnetic solid phase extraction in tandem with liquid-liquid extraction method for determination of four tetracyclines by HPLC with UV detection","volume":"57","author":"Tang","year":"2020","journal-title":"J. Food Sci. Technol."},{"key":"ref_40","doi-asserted-by":"crossref","first-page":"134085","DOI":"10.1016\/j.foodchem.2022.134085","article-title":"Preparation of fatty acid-based ternary deep eutectic solvents: Application for determination of tetracycline residue in water, honey and milk samples by using vortex-assisted microextraction","volume":"400","author":"Lanjwani","year":"2023","journal-title":"Food Chem."},{"key":"ref_41","doi-asserted-by":"crossref","first-page":"1196","DOI":"10.22146\/ijc.64414","article-title":"Pre-concentration and determination of tetracyclines antibiotics residues in water samples using rGO\/Fe3O4 nanocomposite as extraction sorbent","volume":"21","author":"Abdullah","year":"2021","journal-title":"Indones. J. Chem."},{"key":"ref_42","unstructured":"The Commission of the European Communities (2002). Commission decision 2002\/657\/EC of 12 August 2002 implementing council directive 96\/23\/EC concerning the performance of analytical methods and interpretation of results (2002\/657\/EC). Off. J. Eur. Communities, L221, 8\u201336."}],"container-title":["Molecules"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1420-3049\/28\/21\/7421\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,10]],"date-time":"2025-10-10T21:17:28Z","timestamp":1760131048000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1420-3049\/28\/21\/7421"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2023,11,3]]},"references-count":42,"journal-issue":{"issue":"21","published-online":{"date-parts":[[2023,11]]}},"alternative-id":["molecules28217421"],"URL":"https:\/\/doi.org\/10.3390\/molecules28217421","relation":{},"ISSN":["1420-3049"],"issn-type":[{"value":"1420-3049","type":"electronic"}],"subject":[],"published":{"date-parts":[[2023,11,3]]}}}