Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Química, Universidad de La Laguna (ULL), Avenida Astrofísico Francisco Sánchez, s/n. 38206 La Laguna, Tenerife, Spain.
Talanta. 2013 Nov 15;116:695-703. doi: 10.1016/j.talanta.2013.07.060. Epub 2013 Jul 31.
In this manuscript, a new method based on the use of off-line dispersive solid-phase extraction (dSPE) combined with ultra-high performance liquid chromatography with diode-array detection was developed to determine 11 sulfonamide antibiotics (sulfanilamide, sulfacetamide, sulfadiazine, sulfathiazole, sulfamerazine, sulfadimidin, sulfamethoxypyridazine, sulfadoxine, sulfamethoxazole, sulfisoxazole and sulfadimethoxine) in mineral waters with different mineral content. For this purpose, pristine multi-walled carbon nanotubes (MWCNTs) and magnetic-MWCNTs (m-MWCNTs) were used as sorbents. Magnetic nanoparticles were synthesized by means of a solvothermal process, assembled onto CNTs through an "aggregation wrap" mechanism and characterized by scanning electron microscopy. Parameters affecting the extraction such as volume and pH of the sample, amount of sorbent and type and volume of eluent were optimized. Once optimum extraction conditions (250 mL of water at pH 6.0 and elution with 25 mL of MeOH) were obtained, the extraction efficiency of the different carbon nanomaterials was compared. Results demonstrated the higher extraction capacity of pristine MWCNTs with recoveries between 61 and 110% (except for sulfacetamide which ranged between 40 and 53%) and between 22 and 77% for m-MWCNTs. Limits of detection lower than 32 ng/L were achieved for all of the analyzed samples.
在本手稿中，开发了一种基于离线分散固相萃取（dSPE）与二极管阵列检测超高效液相色谱相结合的新方法，用于测定不同矿物质含量矿泉水中的 11 种磺胺类抗生素（磺胺、磺胺醋酰、磺胺嘧啶、磺胺噻唑、磺胺甲噁唑、磺胺二甲嘧啶、磺胺甲氧嘧啶、磺胺多辛、磺胺甲噁唑、磺胺异噁唑和磺胺二甲氧嘧啶）。为此，使用原始多壁碳纳米管（MWCNTs）和磁性多壁碳纳米管（m-MWCNTs）作为吸附剂。通过溶剂热法合成磁性纳米颗粒，通过“聚集包裹”机制组装到 CNTs 上，并通过扫描电子显微镜进行了表征。优化了影响提取的参数，如样品的体积和 pH 值、吸附剂的量以及洗脱液的类型和体积。一旦获得最佳提取条件（pH 6.0 下 250 mL 水和 25 mL MeOH 洗脱），就比较了不同碳纳米材料的提取效率。结果表明，原始 MWCNTs 的提取能力更高，回收率在 61%至 110%之间（除磺胺醋酰在 40%至 53%之间），m-MWCNTs 的回收率在 22%至 77%之间。所有分析样品的检测限均低于 32 ng/L。
