Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Hubei Province, Wuhan, P. R. China.
J Sep Sci. 2019 Mar;42(5):1058-1066. doi: 10.1002/jssc.201801177. Epub 2019 Feb 13.
A novel magnetic adsorbent Fe O /reduced graphene oxide-carbon nanotubes, was prepared by one-pot solvothermal synthesis method. It was characterized by scanning electron microscopy, X-ray powder diffraction and vibrating sample magnetometry. The diameter of Fe O microparticles was about 350 nm, which were covered by carbon nanotubes and reduced graphene oxide sheets, while carbon nanotubes inserted between the reduced graphene oxide sheets effectively prevented their aggregation. The composite had large surface area and good magnetic property, suiting for magnetic solid-phase extraction and the determination of sulfonamides, by coupling with high-performance liquid chromatography. Under the optimized conditions (including extraction time, amount of adsorbent, solution pH, ionic strength and desorption conditions), a good linear was achieved in the concentration range of 5-500 μg/L and the low limits of detection and low limits of quantification were 0.35-1.32 and 1.16-4.40 μg/L, respectively. The enrichment factors were estimated to be 24.72 to 30.15 fold. The proposed method was applied for the detection of sulfonamides in milk sample and the recoveries were 88.4-105.9%, with relative standard deviations of 0.74-5.38%.
一种新型的磁性吸附剂 Fe3O4/还原氧化石墨烯-碳纳米管，通过一步溶剂热合成法制备。通过扫描电子显微镜、X 射线粉末衍射和振动样品磁强计对其进行了表征。Fe3O4 微粒的直径约为 350nm，被碳纳米管和还原氧化石墨烯片所覆盖，而碳纳米管插入在还原氧化石墨烯片之间，有效地防止了它们的聚集。该复合材料具有较大的表面积和良好的磁性，适合通过与高效液相色谱法结合进行磁性固相萃取和磺胺类药物的测定。在优化的条件下（包括萃取时间、吸附剂用量、溶液 pH 值、离子强度和洗脱条件），在 5-500μg/L 的浓度范围内得到了良好的线性关系，检测限和定量限分别为 0.35-1.32μg/L 和 1.16-4.40μg/L。富集因子估计为 24.72 至 30.15 倍。该方法被应用于牛奶样品中磺胺类药物的检测，回收率为 88.4-105.9%，相对标准偏差为 0.74-5.38%。
