College of Medical Technology, Chengdu University of Traditional Chinese Medicine, 1166 Liutai Avenue, Chengdu, Sichuan, 611137, China; Research Center of Analysis and Measurement, Fudan University, 2005 Songhu Road, Shanghai, 200438, China.
College of Medical Technology, Chengdu University of Traditional Chinese Medicine, 1166 Liutai Avenue, Chengdu, Sichuan, 611137, China; Research Center of Analytical Instrumentation, Key Laboratory of Bio-resource and Eco-environment, Ministry of Education, College of Life Sciences, Sichuan University, 29 Jiuyanqiao Wangjiang Road, Chengdu, 610065, China.
J Chromatogr A. 2019 Dec 6;1607:460402. doi: 10.1016/j.chroma.2019.460402. Epub 2019 Jul 26.
Monodispersed magnetic microspheres were synthesized by the magnetization of the aminized polystyrene cores and the subsequent polymerization of allyl glycidyl ether, divinylbenzene and N-vinyl-2-pyrrolidone, which exhibited excellent monodispersity in aqueous solution and high efficiency for allyl-benzodioxoles extraction. Various techniques, including scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FT-IR) and vibrating sample magnetometry (VSM) were employed to characterize the composites. Coupled with gas chromatography-mass spectrometry (GC-MS), a sensitive and simple magnetic solid phase extraction (MSPE) procedure based on the prepared microspheres was established for determination of allyl-benzodioxoles in cola-flavoured drinks. The factors affecting the extraction procedure, such as pH value, adsorbent amount, adsorption time, desorption solution and desorption time were optimized. The developed method was characterized by a high recovery (spiked at 5 μg L, 25 μg L and 250 μg L), a low detection limit (0.05 μg L for safrole and 0.08 μg L for myristicin), a good linearity (correlation coefficients higher than 0.9990 for both) and a satisfactory repeatability (relative standard deviation below 3.7% for both, n = 3). The approach proposed here was confirmed to be fast and reliable for quantitative analysis of allyl-benzodioxoles in cola samples, especially at a trace level.
单分散磁性微球通过氨基化聚苯乙烯核的磁化以及随后的烯丙基缩水甘油醚、二乙烯基苯和 N-乙烯基-2-吡咯烷酮的聚合来合成，在水溶液中表现出极好的单分散性和对烯丙基苯并二恶唑的高效萃取。采用扫描电子显微镜（SEM）、透射电子显微镜（TEM）、傅里叶变换红外光谱（FT-IR）和振动样品磁强计（VSM）等多种技术对复合材料进行了表征。结合气相色谱-质谱（GC-MS），建立了一种基于制备的微球的灵敏、简单的磁性固相萃取（MSPE）方法，用于测定可乐风味饮料中的烯丙基苯并二恶唑。优化了影响萃取过程的因素，如 pH 值、吸附剂用量、吸附时间、解吸溶液和解吸时间。所开发的方法具有较高的回收率（在 5μg/L、25μg/L 和 250μg/L 时进行加标）、较低的检测限（对黄樟素的检测限为 0.05μg/L，对肉豆蔻醚的检测限为 0.08μg/L）、良好的线性（相关系数均高于 0.9990）和令人满意的重复性（两者的相对标准偏差均低于 3.7%，n=3）。该方法快速可靠，可用于可乐样品中烯丙基苯并二恶唑的定量分析，特别是痕量分析。
