Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Campus Fuentenueva s/n, E-18071 Granada, Spain.
Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Campus Fuentenueva s/n, E-18071 Granada, Spain.
Talanta. 2015 Jun 1;138:258-262. doi: 10.1016/j.talanta.2015.03.012. Epub 2015 Mar 12.
An analytical method based on on-line solid-phase extraction coupled to liquid chromatography with photoinduced fluorescence detection has been developed to determine sulfonamides in serum. A home-made setup was used to percolate 3 mL of sample through a solid-phase extraction column. Analytes were retained onto the sorbent by an anion exchange mechanism which ensures an optimum compatibility with the subsequent chromatographic separation using a C-18 column and an on-line photoreactor in order to derivatize sulfonamides, which do not present native fluorescence. The method allowed the determination of 7 sulfonamides in serum samples previously deproteinized in less than 18 min and with limits of detection ranging between 1.8 and 3.6 mg/L. Relative recoveries between 91.5% and 102.1% were obtained with satisfactory precision since relative standard deviations were always below 10.5%.
建立了一种基于在线固相萃取-液相色谱-光诱导荧光检测的分析方法，用于测定血清中的磺胺类药物。采用自制装置将 3 mL 样品通过固相萃取柱进行渗滤。通过阴离子交换机制将分析物保留在吸附剂上，这确保了与随后使用 C-18 柱和在线光反应器进行的色谱分离的最佳兼容性，以便衍生没有天然荧光的磺胺类药物。该方法允许在少于 18 分钟的时间内对血清样品进行去蛋白处理，并测定 7 种磺胺类药物，检测限在 1.8 至 3.6 mg/L 之间。相对回收率在 91.5%至 102.1%之间，精密度令人满意，因为相对标准偏差始终低于 10.5%。
