Gong Sheng-Xiang, Wang Xiao-Li, Liu Wei, Wang Ming-Lin, Wang Xia, Wang Zheng-Wu, Zhao Ru-Song
Key Laboratory for Applied Technology of Sophisticated Analytical Instruments of Shandong Province, Analysis and Test Centre, Shandong Academy of Sciences, Jinan, China.
College of Food Science and Engineering, Shandong Agricultural University, Taian, China.
J Sep Sci. 2017 Apr;40(8):1755-1764. doi: 10.1002/jssc.201601228. Epub 2017 Mar 23.
Aminosilanized magnetic carbon microspheres as a novel adsorbent were designed and fabricated. The adsorbent was used for the magnetic solid-phase extraction of bisphenols at trace levels from environmental water samples before liquid chromatography with tandem mass spectrometry analysis. The structure, surface, and magnetic behavior of the as-prepared aminosilanized magnetic carbon microspheres were characterized by elemental analysis, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, powder X-ray diffraction, and vibrating sample magnetometry. The effects of the experimental parameters were investigated by the Plackett-Burman design, and then the parameters that were significant to the extraction efficiencies were optimized through a response surface methodology. The aminosilanized magnetic carbon microspheres exhibited high adsorption efficiency and selectivity for bisphenols. Under optimal conditions, low limits of detection (0.011-2.22 ng/L), and a wide linear range (2-3 orders of magnitude), good repeatability (4.7-7.8%, n = 5), and reproducibility (6.0-8.3%, n = 3) were achieved. The results demonstrate that the novel adsorbent possesses great potentials in the determination of trace levels of bisphenols in environmental water samples.
设计并制备了氨基硅烷化磁性碳微球作为一种新型吸附剂。该吸附剂用于在液相色谱 - 串联质谱分析之前,从环境水样中磁性固相萃取痕量双酚。通过元素分析、扫描电子显微镜、透射电子显微镜、傅里叶变换红外光谱、粉末X射线衍射和振动样品磁强计对所制备的氨基硅烷化磁性碳微球的结构、表面和磁行为进行了表征。采用Plackett - Burman设计研究了实验参数的影响,然后通过响应面法对萃取效率有显著影响的参数进行了优化。氨基硅烷化磁性碳微球对双酚表现出高吸附效率和选择性。在最佳条件下,实现了低检测限(0.011 - 2.22 ng/L)、宽线性范围(2 - 3个数量级)、良好的重复性(4.7 - 7.8%,n = 5)和重现性(6.0 - 8.3%,n = 3)。结果表明,这种新型吸附剂在测定环境水样中痕量双酚方面具有巨大潜力。