Zhang Wenmin, Lin Mingxia, Wang Meili, Tong Ping, Lu Qiaomei, Zhang Lan
Ministry of Education Key Laboratory for Analytical Science of Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian, 350116, China.
Ministry of Education Key Laboratory for Analytical Science of Food Safety and Biology, Fujian Provincial Key Laboratory of Analysis and Detection Technology for Food Safety, College of Chemistry, Fuzhou University, Fuzhou, Fujian, 350116, China; Testing Center, The Sport Science Research Center, Fuzhou University, Fuzhou, Fujian, 350002, China.
J Chromatogr A. 2017 Jun 23;1503:1-11. doi: 10.1016/j.chroma.2017.04.063. Epub 2017 May 1.
Microcystins (MCs) are cyclic heptapeptide toxins and tumor promoters produced by cyanobacteria, which threaten the health of humans. In this study, magnetic porous β-cyclodextrin polymer (FeO@SiO@P-CDP) was synthesized and characterized by transmission electron microscopy, scanning electron microscopy, energy dispersive X-ray spectrometry, Fourier transform infrared spectrometry, X-ray diffraction, nitrogen adsorption porosimetry and vibrating sample magnetometer. The synthesized FeO@SiO@P-CDP particles were then used for magnetic solid-phase extraction (MSPE) of MCs from environmental water samples, and exhibited excellent extraction performance, especially for MC-RR. Coupled with high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS), a simple, efficient and sensitive method for determination of trace levels of MCs was established. After the optimization of conditions, wide linear ranges (2.0-1000pgmL), good linearity (r≥0.9996) and acceptable repeatability (RSD≤9.4%, n=5) were obtained. The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) for three MCs (MC-LR, MC-RR and MC-YR) were in the range of 1.0-2.0pgmL and 2.0-5.0pgmL, respectively. Typical water samples were analyzed by the developed method, and trace levels of MC-LR and MC-RR were detected. The results demonstrate that the developed method has great potential for the determination of MCs in complicated matrix.
微囊藻毒素（MCs）是蓝藻产生的环状七肽毒素和肿瘤促进剂，威胁着人类健康。在本研究中，合成了磁性多孔β-环糊精聚合物（FeO@SiO@P-CDP），并通过透射电子显微镜、扫描电子显微镜、能量色散X射线光谱、傅里叶变换红外光谱、X射线衍射、氮吸附孔隙率测定法和振动样品磁强计对其进行了表征。然后将合成的FeO@SiO@P-CDP颗粒用于环境水样中MCs的磁性固相萃取（MSPE），并表现出优异的萃取性能，尤其是对MC-RR。结合高效液相色谱-串联质谱（HPLC-MS/MS），建立了一种简单、高效、灵敏的痕量MCs测定方法。条件优化后，获得了宽线性范围（2.0-1000pg/mL）、良好的线性关系（r≥0.9996）和可接受的重复性（RSD≤9.4%，n=5）。三种微囊藻毒素（MC-LR、MC-RR和MC-YR）的检测限（LODs，S/N=3）和定量限（LOQs，S/N=10）分别在1.0-2.0pg/mL和2.0-5.0pg/mL范围内。采用所建立的方法对典型水样进行分析，检测到痕量的MC-LR和MC-RR。结果表明，所建立的方法在复杂基质中MCs的测定方面具有很大的潜力。
