Dong Maofeng, Si Wenshuai, Wang Weimin, Bai Bing, Nie Dongxia, Song Weiguo, Zhao Zhihui, Guo Yirong, Han Zheng
Institute for Agri-food Standards & Testing Technology, Shanghai Academy of Agricultural Sciences, 1000 Jinqi Road, Shanghai, 201403, China.
Institute of Pesticide and Environmental Toxicology, Zhejiang University, Hangzhou, Zhejiang, 310058, China.
Anal Bioanal Chem. 2016 Sep;408(24):6823-31. doi: 10.1007/s00216-016-9809-0. Epub 2016 Jul 30.
Magnetic solid-phase extraction (m-SPE) is a promising sample preparation approach due to its convenience, speed, and simplicity. For the first time, a rapid and reliable m-SPE approach using magnetic multi-walled carbon nanotubes (m-MWCNTs) as the adsorbent was proposed for purification of type A trichothecenes including T-2 toxins (T2), HT-2 toxins (HT-2), diacetoxyscirpenol (DAS), and neosolaniol (NEO) in coix seed. The m-MWCNTs were synthesized by assembling the magnetic nanoparticles (Fe3O4) with MWCNTs by sonication through an aggregation wrap mechanism, and characterized by transmission electron microscope. Several key parameters affecting the performance of the procedure were extensively investigated including extraction solutions, desorption solvents, and m-MWCNT amounts. Under the optimal sample preparation conditions followed by analysis with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), high sensitivity (limit of quantification in the range of 0.3-1.5 μg kg(-1)), good linearity (R (2) > 0.99), satisfactory recovery (73.6-90.6 %), and acceptable precision (≤2.5 %) were obtained. The analytical performance of the developed method has also been successfully evaluated in real coix seed samples. Graphical Abstract Flow chart of determination of type A trichothecenes in coix seed by magnetic solid-phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry.
磁性固相萃取(m-SPE)因其便捷、快速和简单而成为一种很有前景的样品制备方法。首次提出了一种以磁性多壁碳纳米管(m-MWCNTs)为吸附剂的快速可靠的m-SPE方法,用于纯化薏苡仁中包括T-2毒素(T2)、HT-2毒素(HT-2)、二醋酸雪腐镰刀菌烯醇(DAS)和新茄病镰刀菌烯醇(NEO)在内的A型单端孢霉烯族毒素。通过超声处理,利用聚集包裹机制将磁性纳米颗粒(Fe3O4)与多壁碳纳米管组装合成m-MWCNTs,并通过透射电子显微镜对其进行表征。广泛研究了影响该方法性能的几个关键参数,包括萃取溶液、解吸溶剂和m-MWCNT的用量。在最佳样品制备条件下,随后采用超高效液相色谱-串联质谱(UHPLC-MS/MS)进行分析,获得了高灵敏度(定量限在0.3-1.5 μg kg-1范围内)、良好的线性(R (2) > 0.99)、令人满意的回收率(73.6-90.6%)和可接受的精密度(≤2.5%)。所建立方法的分析性能也已在实际薏苡仁样品中成功评估。图摘要 磁性固相萃取结合超高效液相色谱-串联质谱法测定薏苡仁中A型单端孢霉烯族毒素的流程图