Collge of Food Science, Fujian Agriculture and Forestry University, 350002, Fuzhou, Fujian, China.
Fujian Inspection and Research Institute for Product Quality, 350001, Fuzhou, Fujian, China.
J Chromatogr A. 2020 Jul 5;1622:461098. doi: 10.1016/j.chroma.2020.461098. Epub 2020 Apr 28.
In the current study, a novel covalent organic frameworks COF-SCU1 incorporated electrospun nanofibers (PAN@COF-SCU1 nanofibers) was fabricated via a facile electrospinning method and utilized as adsorbent in pipette tip solid-phase extraction (PT-SPE) of tetracycline antibiotics (TCs) from foods. The prepared PAN@COF-SCU1 nanofibers possessed both of the unique characteristics of electrospun nanofibers and COFS-CU1, and thus improving the adsorption capacity of the electrospun nanofibers and preventing the problems of leakage and high pressure caused by directly using the nanosize COFs as adsorbent in PT-SPE. The experiments affected the adsorption and desorption efficiencies, such as the loading ratios of COFS-CU1 in nanofibers, the amount of nanofibers, the matrix pH and desorption solvent, were studied in detail. Eventually, a new pipette tip solid-phase extraction-high performance liquid chromatography (PT-SPE/HPLC) method was proposed for the analysis of three TCs from food. Satisfied linearity for TCs was obtained in the range of 4-70 ng mL. The limits of detection and quantification were ranged from 0.6 to 3 ng mL and from 2 to 10 ng mL, respectively. The interday and intraday precisions (RSD) were all lower than 9%. The proposed PT-SPE/HPLC method was used to determine TCs residues in grass carp and duck samples for the first time. The results could not only explore the availability of PT-SPE in the extraction of TCs in food samples, but also broadened the potential applications of COFs in sample preparation.
在本研究中,通过简便的静电纺丝方法制备了一种新型的共价有机骨架 COF-SCU1 复合静电纺纳米纤维(PAN@COF-SCU1 纳米纤维),并将其用作从食品中提取四环素类抗生素(TCs)的管内固相萃取(PT-SPE)的吸附剂。所制备的 PAN@COF-SCU1 纳米纤维兼具静电纺纳米纤维和 COFS-CU1 的独特特性,从而提高了静电纺纳米纤维的吸附能力,并防止了直接将纳米 COFS 用作 PT-SPE 中的吸附剂时出现的泄漏和高压问题。详细研究了影响吸附和解吸效率的实验因素,如纳米纤维中 COFS-CU1 的负载比、纳米纤维的用量、基质 pH 值和洗脱溶剂等。最终,提出了一种新的管内固相萃取-高效液相色谱(PT-SPE/HPLC)方法,用于分析食品中的三种 TCs。TCs 在 4-70 ng mL 的范围内呈现出满意的线性。检测限和定量限的范围分别为 0.6-3 ng mL 和 2-10 ng mL。日内和日间精密度(RSD)均低于 9%。首次将所提出的 PT-SPE/HPLC 方法用于草鱼和鸭肉样品中 TCs 残留的测定。该结果不仅可以探索 PT-SPE 在食品样品中 TCs 提取中的可用性,还拓宽了 COFs 在样品制备中的潜在应用。