Department of Analytical Chemistry and Food Technology, University of Castilla-La Mancha, 13071 Ciudad Real, Spain.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Jan 15;913-914:12-8. doi: 10.1016/j.jchromb.2012.11.015. Epub 2012 Nov 27.
This work reports the validation of a high precision and accuracy method for the simultaneous determination of letrozole, citalopram and their metabolites in urine by high performance liquid chromatography with fluorescence detection. Dilution (urine:mobile phase, 1:2, v/v) was the only sample preparation step. The separation was carried out in a Kromasil C(18) (150mm×4.6mm) column, and the mobile phase was phosphate buffer 80mM (pH 3.0) and acetonitrile (65:35, v/v) at a flow rate of 1.0mL/min. The analytes were detected at 295nm after excitation at 230nm. Linearity was observed in the range of 1.0-1000ng/mL for letrozole and its metabolite and 2.5-1000ng/mL for citalopram and their metabolites, with limits of detection and quantification between 0.09-1.0 and 0.27-1.65ng/mL, respectively. The precisions were satisfactory with RSDs between 0.17 and 5.71%. The accuracy was studied by spiking three urines from healthy female volunteers, and the recoveries were from 85 to 103%. The method was applied to urine samples from women under treatment for breast cancer and depression diseases.
本工作报道了一种高效液相色谱-荧光检测法同时测定尿液中来曲唑、西酞普兰及其代谢物的精密度和准确度。稀释（尿液：流动相，1:2，v/v）是唯一的样品制备步骤。分离在 Kromasil C(18)（150mm×4.6mm）柱上进行，流动相为 80mM 磷酸盐缓冲液（pH 3.0）和乙腈（65:35，v/v），流速为 1.0mL/min。在 295nm 处检测到 230nm 激发的分析物。来曲唑及其代谢物的线性范围为 1.0-1000ng/mL，西酞普兰及其代谢物的线性范围为 2.5-1000ng/mL，检测限和定量限分别为 0.09-1.0 和 0.27-1.65ng/mL。精密度令人满意，RSD 在 0.17 到 5.71%之间。通过向 3 名健康女性志愿者的尿液中添加标准品来研究准确性，回收率在 85%到 103%之间。该方法应用于乳腺癌和抑郁症患者的尿液样本。
