Department of Analytical Chemistry, University of Tabriz, Iran.
Luminescence. 2012 Jul-Aug;27(4):268-73. doi: 10.1002/bio.1344. Epub 2011 Aug 18.
Optimized conditions, validation and practical applications of a new, rapid and specific fluorometric method for the determination of deferiprone (DFP) in urine and serum samples are reported. The proposed method, which is based on the formation of a luminescent complex with Tb(3+) ion, is evaluated in terms of linearity, accuracy, precision, stability, recovery and limits of detection (LOD) and quantification (LOQ). Under optimum conditions (pH 7.5, [Tb(3+)] = 3 × 10(-4) mol/L, temperature 0 °C and excitation wavelength 295 nm), the relative intensities at 545 nm are linear, with the concentration of DFP in the range 0.072-13 mmol/L for urine and serum samples. The LOD and LOQ, respectively, are calculated to be 0.014 and 0.045 mmol/L for urine and 0.022 and 0.072 mmol/L for serum samples. The intra-day and inter-day values for the precision and accuracy of the proposed method are all < 5%, and the recovery of the method is in the range 97.1-103.8%. The method was applied to human urine and serum samples collected from patients receiving DFP. The results indicated that the method can be successfully applied to the determination of DFP in human urine and serum samples collected for clinical or biopharmaceutical investigations in which simple, rapid, cheap and specific determination methods facilitate and speed up the analytical procedure.
优化条件下,报告了一种新的、快速且特异的荧光法测定尿液和血清中去铁酮(DFP)的条件、验证和实际应用。该方法基于与 Tb(3+)离子形成发光络合物,从线性、准确性、精密度、稳定性、回收率和检测限(LOD)和定量限(LOQ)方面进行了评估。在最佳条件下(pH 7.5,[Tb(3+)] = 3 × 10(-4) mol/L,温度 0 °C,激发波长 295 nm),545 nm 处的相对强度与尿液和血清样品中 DFP 的浓度在 0.072-13 mmol/L 范围内呈线性关系。LOD 和 LOQ 分别计算为尿液 0.014 和 0.045 mmol/L,血清 0.022 和 0.072 mmol/L。该方法的日内和日间精密度和准确度的变异系数均<5%,方法的回收率在 97.1-103.8%范围内。该方法应用于接受 DFP 治疗的患者的尿液和血清样本中。结果表明,该方法可成功应用于收集的人尿液和血清样品中 DFP 的测定,这对于临床或生物制药研究中的简单、快速、廉价和特异的测定方法有利于加快分析程序。