在HPLC-DAD定量前,使用废弃pet衍生的UIO-66作为吸附剂预先浓缩选定的头孢菌素

Andisiwe Bangani , Mthokozisi Mnguni , Thollwana Andretta Makhetha , Elisabete Oliveira , José Luis Capelo-Martínez , Carlos Lodeiro , Philiswa Nosizo Nomngongo
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引用次数: 0

摘要

本研究建立了超声辅助分散固相萃取(UA-DSPE)和高效液相色谱-二极管阵列检测(HPLC-DAD)对不同水样中5种头孢菌素类抗生素的提取、预富集和测定方法。制备了废旧pet衍生物UIO-66作为吸附剂。采用傅里叶变换红外光谱、x射线衍射、高分辨率扫描电镜、透射电镜和能量色散x射线能谱对所制备的吸附剂进行了表征。材料的大表面积、孔体积和微孔性质是保证头孢菌素类抗生素(头孢哌酮、头孢曲松、头孢肽、头孢克洛和头孢西丁)有丰富的活性吸附位点所必需的。采用中心复合设计对影响UA-DSPE方法的因素进行了优化。在优化条件下,线性范围为0.1 ~ 700µg/L,测定系数大于0.99。检测限为0.026 ~ 0.096 μg/L,定量限为0.09 ~ 0.32 μg/L。日内加标回收率为71.4 ~ 99.3%,日内加标回收率为72.6 ~ 99.1%,相对标准偏差小于6%。UA-DSPE/HPLC-DAD方法成功地应用于实际环境样品,如废水和地表水。通过一系列吸附实验研究了废pet衍生UIO-66材料的吸附性能。吸附等温线和动力学表明,Langmuir等温线和拟二级动力学模型解释了吸附过程。废pet衍生UIO-66对目标分析物的最大吸附量为68.3-106 mg/g。上述结果表明,pet衍生的UIO-66材料可作为一种可持续吸附剂用于吸附去除垃圾中的头孢菌素类抗生素。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Preconcentration of selected cephalosporins using waste PET-derived UIO-66 as an adsorbent before HPLC-DAD quantification
In this work, a method for the extraction, preconcentration and determination of five different cephalosporin antibiotics in various water samples using ultrasound-assisted dispersive solid-phase extraction (UA-DSPE) and high-performance liquid chromatography coupled with diode-array detection (HPLC-DAD) was developed. The waste PET-derived UIO-66 was prepared and used as an adsorbent. The prepared adsorbent was characterised using Fourier transform infrared spectroscopy, X-ray diffraction, high-resolution scanning electron microscopy, transmission electron microscopy and energy-dispersive X-ray spectroscopy. The large surface area, pore volume, and microporous nature of the material were necessary to ensure there were abundant active sorption sites for the cephalosporin antibiotics (cefoperazone, ceftriaxone, cephalothin, cefaclor and cefoxitin). The factors affecting the UA-DSPE method were optimised using a central composite design. Under optimised conditions, wide linearity ranging from 0.1–700 µg/L with the determination coefficients greater than 0.99. The limits of detection and quantification were in the range of 0.026–0.096 μg/L and 0.09–0.32 μg/L, respectively. The intraday and interday spiked recoveries were 71.4–99.3 % and 72.6–99.1 %, respectively, with the relative standard deviation values less than 6 %. The UA-DSPE/HPLC-DAD method was successfully applied to real environmental samples such as wastewater and surface water. The adsorptive performance of the waste PET-derived UIO-66 material was investigated using a series of adsorption experiments. The adsorption isotherms and kinetics indicated that the Langmuir isotherm and pseudo-second-order kinetic models explained the adsorption process. The maximum adsorption capacities for the target analytes using waste PET-derived UIO-66 ranged from 68.3–106 mg/g. These results demonstrated that the waste PET-derived UIO-66 material could be used as a sustainable adsorbent for the adsorptive removal of cephalosporin antibiotics from waster.
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