Villar Navarro M, Ramos Payán M, Fernández-Torres R, Bello López M A
Department of Analytical Chemistry, Faculty of Chemistry, University of Seville, Seville, Spain.
Biomed Chromatogr. 2013 Feb;27(2):246-53. doi: 10.1002/bmc.2783. Epub 2012 Jul 3.
In this paper two applications of three-phase HF-LPME for the determination of pharmaceuticals in human urine are proposed: a capillary electrophoresis with a photodiode array detection method for the analysis of seven nonsteroidal anti-inflammatory drugs (NSAIDs) and a high-performance liquid chromatographic with photo diode array and fluorescence detection method for the determination of four sulfonamides and their corresponding N(4)-acetyl-metabolites. Q3/2 Accurel® polypropylene hollow fibers were used for both procedures. Dihexyl ether was used as the supported liquid membrane for the determination of anti-inflammatories and 1-octanol for sulfonamides. An aqueous solution (pH 12) was used in both procedures as the acceptor phase and as the donor phase an aqueous solution (pH 2), and a 2 M Na(2)SO(4) aqueous solution (pH 4) was used for the determination of the anti-inflammatories and sulfonamides. The detection limits obtained were between 0.25 (naproxen) and 0.86 ng/mL (aceclofenac) for the determination of anti-inflammatories and 7 × 10(-4) (sulfamethoxazole) and 0.048 ng/mL (N(4)-acetyl-sulfamethazine) for sulfonamides. The method was successfully applied to the determination of the analytes in human urine.
本文提出了三相高频-液相微萃取在测定人尿中药物的两种应用：一种是采用光电二极管阵列检测的毛细管电泳法分析七种非甾体抗炎药（NSAIDs），另一种是采用光电二极管阵列和荧光检测的高效液相色谱法测定四种磺胺类药物及其相应的N(4)-乙酰代谢物。两种方法均使用Q3/2 Accurel®聚丙烯中空纤维。测定抗炎药时，使用二己醚作为支撑液膜，测定磺胺类药物时使用1-辛醇。两种方法均使用pH 12的水溶液作为接受相，pH 2的水溶液作为供体相，测定抗炎药和磺胺类药物时使用2 M Na(2)SO(4)水溶液（pH 4）。测定抗炎药时获得的检测限在0.25（萘普生）至0.86 ng/mL（醋氯芬酸）之间，测定磺胺类药物时检测限在7×10(-4)（磺胺甲恶唑）至0.048 ng/mL（N(4)-乙酰磺胺二甲嘧啶）之间。该方法成功应用于人尿中分析物的测定。
