Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC, Brazil.
J Chromatogr A. 2010 Oct 15;1217(42):6449-54. doi: 10.1016/j.chroma.2010.08.030. Epub 2010 Aug 24.
A sensitive and precise analysis using hollow fiber renewal liquid membrane (HFRLM) extraction followed by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) is described for determination of five sulfonamides in honey samples. In this procedure, the organic solvent introduced directly into the sample matrix extracts the sulfonamides and carries them over the polypropylene porous membrane. An organic solvent is immobilized inside the polypropylene porous membrane, leading to a homogeneous phase. The stripping phase at higher pH in the lumen of the membrane promotes the ionization of the target compounds releasing them to this phase. The most important parameters affecting the extraction efficiency were optimized by multivariable designs (pH and sample mass, pH and buffer for stripping phase, extraction temperature and time, type and volume of extractor solvent and use of salt to saturate the sample). Detection limits in the range of 5.1-27.4 μg kg(-1) and linearity coefficient of correlation higher than 0.987 were obtained for the target analytes. The results obtained for the proposed method show that HFRLM-LC-MS/MS can be used for determination of the five sulfonamides studied in honey samples with excellent precision, accuracy, practicality and short analysis time.
采用中空纤维更新液膜（HFRLM）萃取，结合高效液相色谱-串联质谱（LC-MS/MS），建立了一种灵敏、准确的检测方法，用于测定蜂蜜样品中的五种磺胺类药物。在该方法中，有机溶剂直接引入样品基质中，提取磺胺类药物并携带它们通过聚丙烯多孔膜。有机溶剂固定在聚丙烯多孔膜内，形成均相。膜内腔中较高 pH 值的洗脱相促进了目标化合物的电离，将其释放到该相中。通过多变量设计（pH 和样品质量、pH 和洗脱相缓冲液、萃取温度和时间、萃取溶剂的类型和体积以及盐的使用以饱和样品）优化了影响萃取效率的最重要参数。对于目标分析物，检测限在 5.1-27.4μgkg(-1)范围内，相关性系数高于 0.987。该方法具有良好的精密度、准确度、实用性和较短的分析时间，可用于蜂蜜样品中五种磺胺类药物的测定。
