Hertzog Gabriel I, Soares Karina L, Caldas Sergiane S, Primel Ednei G
Post-graduate Program in Technological and Environmental Chemistry, Escola de Química e Alimentos, Laboratório de Análise de Compostos Orgânicos e Metais (LACOM), Universidade Federal do Rio Grande, Av. Itália, km 8, Rio Grande, Rio Grande do Sul state, 96203-900, Brazil.
Anal Bioanal Chem. 2015 Jun;407(16):4793-803. doi: 10.1007/s00216-015-8685-3. Epub 2015 Apr 25.
A procedure based on vortex-assisted matrix solid-phase dispersion (MSPD) for the extraction of 15 pharmaceuticals from fish samples with determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was validated. Florisil, C18, diatomaceous earth, chitin, and chitosan were evaluated as solid supports. Best results were obtained with 0.5 g of diatomaceous earth, 0.5 g of sodium sulfate, and 5 mL of methanol. Analytical recoveries ranged from 58 to 128 % with relative standard deviation (RSD) lower than 15 %. Limit of quantification (LOQ) values for the 15 compounds ranged from 5 to 1000 ng g(-1). The method under investigation has shown to be a simple and fast extraction tool with minimum instrumentation and low amount of reagent, resulting in method low cost. Besides, alternative materials, such as chitin and chitosan, which were applied to the dispersion step for the first time, were found to be interesting alternatives.
一种基于涡旋辅助基质固相分散（MSPD）从鱼类样品中提取15种药物并通过液相色谱-串联质谱（LC-MS/MS）进行测定的方法得到了验证。对弗罗里硅土、C18、硅藻土、甲壳素和壳聚糖作为固相载体进行了评估。使用0.5 g硅藻土、0.5 g硫酸钠和5 mL甲醇获得了最佳结果。分析回收率在58%至128%之间，相对标准偏差（RSD）低于15%。15种化合物的定量限（LOQ）值在5至1000 ng g(-1)之间。所研究的方法已证明是一种简单快速的提取工具，所需仪器最少且试剂用量少，从而使方法成本较低。此外，首次应用于分散步骤的甲壳素和壳聚糖等替代材料被发现是有趣的替代品。
