Du Li-Jing, Yi Ling, Ye Li-Hong, Chen Yu-Bo, Cao Jun, Peng Li-Qing, Shi Yu-Ting, Wang Qiu-Yan, Hu Yu-Han
College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, 310036, China.
Drug Clinical Trial Institution, The First Afliated Hospital of Soochow University, Suzhou, 215006, China.
J Chromatogr A. 2018 Feb 16;1537:10-20. doi: 10.1016/j.chroma.2018.01.005. Epub 2018 Jan 3.
A simple and effective method of miniaturized solid-phase extraction (mini-SPE) was developed for the simultaneous purification and enrichment of macrolide antibiotics (MACs) (i.e. azithromycin, clarithromycin, erythromycin, lincomycin and roxithromycin) from honey and skim milk. Mesoporous MCM-41 silica was synthesized and used as sorbent in mini-SPE. Several key parameters affecting the performance of mini-SPE procedure were thoroughly investigated, including sorbent materials, amount of sorbent and elution solvents. Under the optimized condition, satisfactory linearity (r > 0.99), acceptable precision (RSDs, 0.3-7.1%), high sensitivity (limit of detection in the range of 0.01-0.76 μg/kg), and good recoveries (83.21-105.34%) were obtained. With distinct advantages of simplicity, reliability and minimal sample requirement, the proposed mini-SPE procedure coupled with ultrahigh performance liquid chromatography and quadrupole time-of-flight tandem mass spectrometry could become an alternative tool to analyze the residues of MACs in complex food matrixes.
开发了一种简单有效的小型化固相萃取（mini-SPE）方法，用于同时从蜂蜜和脱脂牛奶中纯化和富集大环内酯类抗生素（MACs）（即阿奇霉素、克拉霉素、红霉素、林可霉素和罗红霉素）。合成了介孔MCM-41硅胶并将其用作mini-SPE中的吸附剂。深入研究了影响mini-SPE程序性能的几个关键参数，包括吸附剂材料、吸附剂用量和洗脱溶剂。在优化条件下，获得了令人满意的线性（r > 0.99）、可接受的精密度（RSDs，0.3-7.1%）、高灵敏度（检测限在0.01-0.76 μg/kg范围内）和良好的回收率（83.21-105.34%）。所提出的mini-SPE程序结合超高效液相色谱和四极杆飞行时间串联质谱，具有操作简单、可靠性高和样品需求量少的显著优点，可成为分析复杂食品基质中MACs残留的替代工具。
