Yu Wanqin, Jia Jingwen, Shi Jinmei, Shi Hongmei, Yang Lixin
Hebei Center for Disease Control and Prevention, Shijiazhuang, 050021, China; Key Laboratory of Environment and Human Health of Hebei Province; School of Public Health, Hebei Medical University, Shijiazhuang 050017, China.
Hebei Center for Disease Control and Prevention, Shijiazhuang, 050021, China.
Talanta. 2023 Mar 1;254:124181. doi: 10.1016/j.talanta.2022.124181. Epub 2022 Dec 8.
A magnetic graphene oxide (GO/FeO) nanocomposite was synthesized in one step by a chemical coprecipitation method, which was further used for magnetic solid-phase extraction (MSPE). This study aimed to combine GO/FeO with ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to detect the nitroimidazoles (NDZs) and their three major metabolites in honey samples. GO/FeO was characterized by transmission electron microscopy (TEM), Fourier transform-infrared (FT-IR) spectroscopy, and magnetic property measurement system (MPMS), and the influencing parameters such as adsorbent amount, pH of the dissolved sample solution, sample volume, type and volume of the eluent, shaking speed, and adsorption and desorption time were optimized. Under the optimized conditions, the limits of detection (LOD) and quantitation (LOQ) of the method were 0.003-0.08 μg kg and 0.009-0.3 μg kg, respectively, with good linearity reported in the range of 0.5-20 μg kg (R ≥ 0.9991). The average recoveries of 10 analytes were in the range of 66.0%-90.8% with relative standard deviations (RSD) lower than 6.9% (n = 6). The preparation of GO/FeO and the extraction process were convenient and rapid, and consumed small amounts of organic solvents. The optimized method was successfully applied for extracting NDZs and their three major metabolites from honey samples with good accuracy.
采用化学共沉淀法一步合成了磁性氧化石墨烯（GO/FeO）纳米复合材料，并将其进一步用于磁性固相萃取（MSPE）。本研究旨在将GO/FeO与超高效液相色谱-串联质谱（UPLC-MS/MS）联用，检测蜂蜜样品中的硝基咪唑类药物（NDZs）及其三种主要代谢物。通过透射电子显微镜（TEM）、傅里叶变换红外（FT-IR）光谱和磁性测量系统（MPMS）对GO/FeO进行了表征，并对吸附剂用量、溶解样品溶液的pH值、样品体积、洗脱剂类型和体积、振荡速度以及吸附和解吸时间等影响参数进行了优化。在优化条件下，该方法的检测限（LOD）和定量限（LOQ）分别为0.003 - 0.08 μg/kg和0.009 - 0.3 μg/kg，在0.5 - 20 μg/kg范围内具有良好的线性关系（R≥0.9991）。10种分析物的平均回收率在66.0% - 90.8%之间，相对标准偏差（RSD）低于6.9%（n = 6）。GO/FeO的制备及萃取过程简便快速，且有机溶剂消耗少。该优化方法成功应用于蜂蜜样品中NDZs及其三种主要代谢物的提取，准确性良好。
