title: Determination of fluoroquinolone antibiotics via ionic-liquid-based, salt-induced, dual microextraction in swine feed.
abstract: In conventional microextraction procedures, the disperser (organic solvent or ionic liquid) is left in the aqueous phase and discarded after finishing the microextraction process. Because the disperser is water-soluble, it results in low extraction recovery for polar compounds. In this investigation, an ionic-liquid-based microextraction (ILBME) was integrated with salting-out assisted liquid-liquid microextraction (SALLME) to build an ionic-liquid-based, salt-induced, dual microextraction (ILSDME) for isolation of five fluoroquinolone antibiotics (FQs) with high polarity (log P, -1.0 to 1.0). The proposed ILSDME method incorporates a dual microextraction by converting the disperser in the ILBME to the extractor in the SALLME. Optimization of key factors was conducted by integrating single-factor experiments and central composite design. The optimized experimental parameters were 80 μL [C8MIM][PF6] as extractor, 505 μL acetone as disperser, pH = 2.0, 4.1 min extraction time, and 4.2 g of Na2SO4. Under optimized conditions, high ERs (90.6-103.2 %) and low LODs (0.07-0.61 μg kg(-1)) were determined for five FQs in swine feed. Experimental precision based on RSDs was 1.4-5.2 % for intra-day and 2.4-6.9 % for inter-day analyses. The combination of ILBME with SALLME increased FQ recoveries by 15-20 % as compared with SALLME, demonstrating that the ILSDME method can enhance extraction efficiency for polar compounds compared to single-step microextraction. Therefore, the ILSDME method developed in this study has wide application for pretreatment of moderately to highly polar pollutants in complex matrices. Graphical Abstract A dual microextraction was developed by integrating ionic-liquid-based microextraction with salting-out assisted liquid-liquid microextraction for isolation of five fluoroquinolone antibiotics (FQs) with high polarity (log P = -1.0 to 1.0). The principle of dual microextraction is based on converting the remaining disperser from the first microextraction into an extractor in the second microextraction. Single-factor experiment and central composite design were applied for optimizing operational parameters using 3D response surfaces and contour lines. Under optimized conditions, the method provided high extraction recoveries and low LODs for five FQs in swine feed. The prominent advantage of the dual microextraction is rapid and highly efficient extraction of moderately to highly polar fluoroquinolones from complex matrices.
authors.affiliation: College of Life Sciences, Wenzhou Medical University, Wenzhou, Zhejiang, 325035, China.
authors.forename: Huili
authors.initials: H
authors.lastname: Wang
authors.affiliation: College of Marine Life, Ocean University of China, Qingdao, Shandong, 266000, China.
authors.forename: Ming
authors.initials: M
authors.lastname: Gao
authors.affiliation: Key Laboratory of Watershed Sciences and Health of Zhejiang Province, Wenzhou Medical University, Wenzhou, Zhejiang, 325035, China.
authors.forename: Jiajia
authors.initials: J
authors.lastname: Gao
authors.affiliation: Key Laboratory of Watershed Sciences and Health of Zhejiang Province, Wenzhou Medical University, Wenzhou, Zhejiang, 325035, China.
authors.forename: Nana
authors.initials: N
authors.lastname: Yu
authors.affiliation: Key Laboratory of Watershed Sciences and Health of Zhejiang Province, Wenzhou Medical University, Wenzhou, Zhejiang, 325035, China.
authors.forename: Hong
authors.initials: H
authors.lastname: Huang
authors.affiliation: Key Laboratory of Watershed Sciences and Health of Zhejiang Province, Wenzhou Medical University, Wenzhou, Zhejiang, 325035, China.
authors.forename: Qing
authors.initials: Q
authors.lastname: Yu
authors.affiliation: Key Laboratory of Watershed Sciences and Health of Zhejiang Province, Wenzhou Medical University, Wenzhou, Zhejiang, 325035, China. zjuwxd@163.com.
authors.forename: Xuedong
authors.initials: X
authors.lastname: Wang
mesh_terms: D000821:Animal Feed / Q000032:analysis*; D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis* / Q000302:isolation & purification; D024841:Fluoroquinolones / Q000032:analysis* / Q000302:isolation & purification; D052578:Ionic Liquids / Q000737:chemistry*; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000379:methods*; D012492:Salts / Q000737:chemistry; D013552:Swine
chemical_list: D000900:Anti-Bacterial Agents; D024841:Fluoroquinolones; D052578:Ionic Liquids; D012492:Salts
keywords: Central composite design; Fluoroquinolone antibiotics; Ionic-liquid-based salt-induced dual microextraction (ILSDME); Polar pollutants; Swine feed