State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-products, State Key Laboratory Base of Novel Functional Materials and Preparation Science, School of Materials Science & Chemical Engineering, Ningbo University, Ningbo, Zhejiang 315211, China.
Ningbo Zhongjin Petrochemical Co., Ltd.(,) Ningbo, 315040, China.
J Chromatogr A. 2022 Jan 4;1661:462719. doi: 10.1016/j.chroma.2021.462719. Epub 2021 Nov 29.
In this work, porous electrospun microfibers (PEMFs) were prepared using a polyimide/polyvinylpyrrolidone/polyethylene glycol (PI/PVP/PEG) solution mixture with coaxial ultrasonic water vapor spraying. After removing PVP and PEG by ultrasonic water washing, the PEMFs were successfully demonstrated as adsorbents for solid phase extraction (SPE). Most non-porous electrospun nanofibers are hundreds of nanometers in diameter, with a specific surface area of dozens of square meters per gram. In contrast, the diameter of the as-prepared PEMFs was tuned between 3 and 8 μm, the specific surface area was 76 mg and the pore size was ca 25 nm. Therefore, the flow resistance of the PEMF-SPE cartridges was similar to those of conventional commercial SPE cartridges, and much lower than those of SPE cartridges packed with electrospun nanofibers. Using the PEMF-SPE cartridges with ultra-performance liquid chromatography-fluorescence detector (UPLC-FLD), five fluoroquinolones (FQs) in tap water, egg and milk samples were extracted and quantified successfully. After optimizing the extraction conditions, FQs in water samples were extracted and eluted with high recoveries of 84.8-114.8%. The inter-batch and intra-batch relative standard deviation (RSD) values for the FQs were in the range of 1.9-9.5% (n=3), and the limits of detection were between 0.0024-0.014 μg L. The method was linear in the concentration range of 0.005-10 μg L. The reliability of the developed method was validated by analyzing tap water, egg and milk samples, and the recovery values were found to be in the range of 74.8-116.6% under the optimized conditions.
在这项工作中，采用聚酰亚胺/聚乙烯吡咯烷酮/聚乙二醇（PI/PVP/PEG）溶液混合物，通过同轴超声水蒸气喷射法制备了多孔静电纺微纤维（PEMFs）。通过超声水洗去除 PVP 和 PEG 后，成功地将 PEMFs 用作固相萃取（SPE）的吸附剂。大多数无孔静电纺纳米纤维的直径为数百纳米，比表面积为每克几十平方米。相比之下，所制备的 PEMFs 的直径在 3 到 8 μm 之间可调，比表面积为 76 mg，孔径约为 25 nm。因此，PEMF-SPE 小柱的流动阻力与传统商用 SPE 小柱相似，远低于填充有静电纺纳米纤维的 SPE 小柱。使用带有超高效液相色谱-荧光检测器（UPLC-FLD）的 PEMF-SPE 小柱，成功地从自来水中、鸡蛋和牛奶样品中提取和定量了五种氟喹诺酮类（FQs）。在优化了提取条件后，水样中的 FQs 以高回收率（84.8-114.8%）被提取和洗脱。FQs 在批内和批间的相对标准偏差（RSD）值在 1.9-9.5%（n=3）范围内，检测限在 0.0024-0.014μg L 之间。该方法在 0.005-10μg L 的浓度范围内呈线性。通过分析自来水、鸡蛋和牛奶样品验证了所建立方法的可靠性，在优化条件下，回收率在 74.8-116.6%范围内。
