Rodríguez Flores J, Salcedo A M Contento, Llerena M J Villaseñor, Fernández L Muñoz
Department of Analytical Chemistry and Foods Technology, University of Castilla-La Mancha, 13071 Ciudad Real, Spain.
J Chromatogr A. 2008 Mar 28;1185(2):281-90. doi: 10.1016/j.chroma.2008.01.067. Epub 2008 Jan 31.
A new micellar electrokinetic chromatographic method has been developed to analyse human urine samples containing a combination of a drug used for the treatment of breast cancer (letrozole), an antidepressant (citalopram) and their main metabolites. Best results were obtained by using 15 mM borate buffer (pH 9.2) containing 20 mM sodium dodecyl sulphate and 12% (v/v) 2-propanol as the background electrolyte. The separation was performed through a fused silica capillary at 40 degrees C with the application of 6s (3.45 kPa) of hydrodynamic injection and 30 kV of separation voltage. Detection wavelength was 240 nm. Under these conditions, the migration times for all the studied compounds were ranged between 3.0 and 8.0 min. Linearity ranges were determined as 0.4-5.0 microg/mL for all the compounds. Detection limits between 12.5 and 25 ng/mL were determined in urine samples. According to the validation study, the developed method has been proven to be accurate, precise, sensitive, specific, rugged and robust. This method has been used to determine letrozole, citalopram and their metabolites in human urine at clinical levels. Prior to determination, the samples are purified and enriched by means of an extraction-preconcentration step with a preconditioned C(18) cartridge and by eluting the compounds with methanol. The developed method was applied to the determination of these analytes in three urine samples from patients undergoing treatment with letrozole or citalopram.
已开发出一种新型胶束电动色谱法，用于分析含有用于治疗乳腺癌的药物（来曲唑）、一种抗抑郁药（西酞普兰）及其主要代谢物组合的人类尿液样本。使用含有20 mM十二烷基硫酸钠和12%（v/v）异丙醇的15 mM硼酸盐缓冲液（pH 9.2）作为背景电解质可获得最佳结果。分离通过熔融石英毛细管在40℃下进行，采用6s（3.45 kPa）的流体动力进样和30 kV的分离电压。检测波长为240 nm。在这些条件下，所有研究化合物的迁移时间在3.0至8.0分钟之间。所有化合物的线性范围确定为0.4 - 5.0 μg/mL。尿液样本中的检测限在12.5至25 ng/mL之间。根据验证研究，所开发的方法已被证明准确、精密、灵敏、特异、耐用且稳健。该方法已用于测定临床水平人类尿液中的来曲唑、西酞普兰及其代谢物。在测定之前，通过用预处理的C(18)柱进行萃取 - 预浓缩步骤并使用甲醇洗脱化合物来对样品进行纯化和富集。所开发的方法应用于测定来自接受来曲唑或西酞普兰治疗患者的三个尿液样本中的这些分析物。
