分散固相萃取-高效液相色谱-串联质谱法测定蔬菜中17种喹诺酮类药物残留

建立了一种快速、高效、准确的同时测定蔬菜中恩诺沙星、环丙沙星、氧氟沙星、培氟沙星、诺氟沙星、洛美沙星、氟甲喹、恶喹酸、马波沙星、沙拉沙星、达氟沙星、双氟沙星、氟罗沙星、西诺沙星、伊诺沙星、萘啶酸、奥比沙星与吡哌酸等17种喹诺酮类药物残留的分散固相萃取-高效液相色谱-串联质谱方法（dSPE-HPLC-MS/MS）。采用自制的纳米TiO₂修饰COFs材料为dSPE吸附剂,一步实现样品净化;目标分析物在Shim-pack XR-ODS II （150 mm×2.0 mm i.d., 2.2μm）色谱柱上以乙腈和含有0.1%甲酸的水溶液为流动相进行分离,在电喷雾离子源（ESI）正离子多反应监测（MRM）模式下进行检测。17种喹诺酮类药物在0.2μg/kg～100μg/kg范围内具有良好的线性（r²>0.9990）,检出限为0.033μg/kg～0.23μg/kg,最低定量限为0.11μg/kg～0.76μg/kg, RSDs为2.6%～7.3%,加标回收率为76.9%～118%。本法可用于蔬菜中17种喹诺酮类药物残留的快速筛查与确证分析。

Simultaneous analysis of 17 quinolones in vegetables by HPLC-MS/MS with dispersive solid phase extraction

Samples were purified in one step by dSPE with nano-titania functionalized covalent organic frameworks as sorbent. Chromatographic separation of the 17 quinolones was performed on a Shim-pack XR-ODS II(150 mm×2.0 mm i.d., 2.2 μm). The separation could be completed by gradient elution with acetonitrile-formic acid(0.1%, v/v) aqueous solution as mobile phase, using electrospray ion source(ESI) in multiple reaction monitoring(MRM) mode. Linearities of the 17 quinolones were in the range of 0.2 μg/kg—100 μg/kg, with determination coefficients(r;) higher than 0.9990. The limits of detection(LODs) were in the range of 0.033 μg/kg—0.23 μg/kg, and the limits of quantification(LOQs) were between 0.11 μg/kg and 0.76 μg/kg. The relative standard deviations(RSDs) were in the range of 2.6%—7.3%, and recoveries were between 76.9% and 118%. The method can be applied to routine analyses for determination of the 17 quinolones in vegetables.