Guangxi Key Laboratory of Electrochemical and Magnetochemical Functional Materials, College of Chemistry and Bioengineering, Guilin University of Technology, Guilin, 541004, Guangxi, China.
Key Laboratory of Theoretical Organic Chemistry and Function Molecule of Ministry of Education, School of Chemistry and Chemical Engineering, Hunan University of Science and Technology, Xiangtan, 411201, Hunan, China.
Anal Bioanal Chem. 2019 Apr;411(10):2239-2248. doi: 10.1007/s00216-019-01660-1. Epub 2019 Feb 21.
In this work, a novel FeO@Cu(btc)-embedded polymerized high internal phase emulsion (FeO@HKUST-1-polyHIPE) monolithic cake was synthesized, characterized and used as an adsorbent in the magnetic stir cake sorptive extraction (MSCSE) and determination of tetracycline antibiotics (TCs) in food samples by a combination of with high-performance liquid chromatography-fluorescence detection (HPLC-FLD). The prepared FeO@HKUST-1-polyHIPE monolithic composites displayed a strong extraction ability and high column capacity due to enhanced interactions such as π-π interactions, hydrogen bonding, and electrostatic interactions. The extraction and desorption conditions were evaluated, and the calibration curves of four spiked TCs were linear (R ≥ 0.9991) in the range from 20 to 800 ng mL for milk and egg samples, and 20 to 800 ng g for chicken muscle and kidney samples. The limits of detection and the limits of quantification of the four TCs by using the proposed MSCSE-HPLC-FLD method were in the range of 1.9-4.6 and 5.5-13.9 ng mL for milk and egg samples, and 1.8-3.7 and 5.3-13.0 ng g for chicken muscle and kidney samples, respectively. The recoveries of the target TCs from spiked food samples were in the range from 86.6 to 110.7% with relative standard deviations lower than 7.0%. The proposed method was successfully applied for the determination of these four TCs in milk, egg, chicken muscle, and kidney samples.
在这项工作中，合成了一种新型的 FeO@Cu(btc)-嵌入聚合高内相乳液（FeO@HKUST-1-聚合 HIPE）整体蛋糕，并对其进行了表征，然后将其用作磁性搅拌蛋糕吸附萃取（MSCSE）和高效液相色谱-荧光检测（HPLC-FLD）联用测定食品样品中四环素类抗生素（TCs）的吸附剂。由于增强了π-π相互作用、氢键和静电相互作用等相互作用，所制备的 FeO@HKUST-1-聚合 HIPE 整体复合材料表现出较强的萃取能力和较高的柱容量。评估了萃取和洗脱条件，并在牛奶和鸡蛋样品中，四个加标 TCs 的校准曲线在 20 至 800ng mL 范围内呈线性（R≥0.9991），在鸡肉和肾脏样品中在 20 至 800ng g 的范围内呈线性。使用所提出的 MSCSE-HPLC-FLD 方法测定四种 TCs 的检出限和定量限范围分别为牛奶和鸡蛋样品中的 1.9-4.6 和 5.5-13.9ng mL，鸡肉和肾脏样品中的 1.8-3.7 和 5.3-13.0ng g。从加标食品样品中回收的目标 TCs 的回收率在 86.6%至 110.7%之间，相对标准偏差低于 7.0%。该方法成功应用于牛奶、鸡蛋、鸡肉和肾脏样品中这四种 TCs 的测定。
