Analytical Chemistry Division, Department of Chemistry, Lomonosov Moscow State University, Leninskie Gory, 1/3, Moscow, 119991, Russia; Central Scientific Methodological Veterinary Laboratory, Orangereynaya st., 23, 111622, Moscow, Russia.
Analytical Chemistry Division, Department of Chemistry, Lomonosov Moscow State University, Leninskie Gory, 1/3, Moscow, 119991, Russia.
Talanta. 2021 Aug 1;230:122310. doi: 10.1016/j.talanta.2021.122310. Epub 2021 Mar 16.
In this study, 5-nitro-2-furaldehyde (5-NFA) was proposed as a new derivatizing agent for nitrofuran metabolites. It reacts with nitrofuran metabolites producing the parent nitrofurans (furazolidone, furaltadone, nitrofurantoin, and nitrofurazone). Magnetic hypercrosslinked polystyrene (HCP/FeO) was first used for magnetic solid phase extraction (MSPE) clean-up before the determination of nitrofuran metabolite derivatives in honey via LC-MS/MS. Main parameters affecting the derivatization and MSPE efficiency were investigated in detail and the optimal conditions were found. The method was validated using honey spiked with the four metabolites at 1, 2 and 200 μg kg. Recoveries of >85% were achieved for the all analytes. The matrix calibration curve was fitted with the correlation coefficient (R) > 0.99 in the range of 1-200 μg kg. Precision values expressed as relative standard deviation (RSD) were <12% and <15% for intra-day and inter-day precision, respectively. The limits of detection (LODs) for the nitrofuran metabolites were of 0.1-0.3 μg kg and the limits of quantitation (LOQs) were of 0.3-1.0 μg kg. The proposed LC-MS/MS method was applied to the analysis of real honey samples.
在这项研究中，5-硝基糠醛（5-NFA）被提议作为一种新的硝呋喃代谢物衍生化试剂。它与硝呋喃代谢物反应，生成母体硝基呋喃（呋喃唑酮、呋喃它酮、呋喃妥因和呋喃唑酮）。首次使用磁性超交联聚苯乙烯（HCP/FeO）进行磁固相萃取（MSPE）净化，然后通过 LC-MS/MS 测定蜂蜜中的硝呋喃代谢物衍生物。详细研究了影响衍生化和 MSPE 效率的主要参数，并找到了最佳条件。该方法采用蜂蜜中添加四种代谢物（1、2 和 200μg/kg）进行验证。所有分析物的回收率均大于 85%。在 1-200μg/kg 的范围内，基质校准曲线的相关系数（R）大于 0.99。日内和日间精密度的相对标准偏差（RSD）分别小于 12%和 15%。硝呋喃代谢物的检出限（LOD）为 0.1-0.3μg/kg，定量限（LOQ）为 0.3-1.0μg/kg。所提出的 LC-MS/MS 方法应用于实际蜂蜜样品的分析。
