Department of Chemistry, Tunghai University, Taichung, Taiwan.
J Sep Sci. 2012 Mar;35(5-6):681-7. doi: 10.1002/jssc.201100824. Epub 2012 Jan 24.
A simple, rapid and sensitive CE-fluorescence (FL) detection method for the analysis of alendronate (ALEN), a bisphosphonate drug, has been developed. Using a buffer solution of 20 mM sodium phosphate (pH 10.0) and a voltage of 24 kV, separation of ALEN in a 55-cm length (35-cm effective length) capillary was achieved in 5 min. FL detection of ALEN was performed via pre-column derivatization with 2,3-naphthalene dicarbox-yaldehyde (NDA). Linear correlation (r=0.9981, n=6) between FL intensity and analyte concentration was obtained in the range of 7-200 ng/mL ALEN. The developed CE-FL method was applied to the analysis of ALEN in human urine and plasma samples. In order to eliminate the interfering matrix components, SPE using magnetic Fe(3) O(4) @Al(2) O(3) nanoparticles as solid sorbents was employed to clean the biological fluids before CE-FL analysis. The linear ranges of ALEN in urine and plasma were 5-100 ng/mL (r = 0.9982, n = 7) and 5-70 ng/mL (r = 0.9954, n = 7), respectively. The LOD and LOQ in both urine and plasma samples were 1.5 and 5 ng/mL ALEN, respectively. Total analysis time including sample pre-treatment and CE separation was less than 1.5 h.
一种简单、快速和灵敏的毛细管电泳-荧光（FL）检测法已被开发用于分析双膦酸盐药物阿仑膦酸钠（ALEN）。在 20mM 磷酸钠（pH 10.0）缓冲溶液和 24kV 电压下，在 55cm 长（35cm 有效长度）的毛细管中，ALEN 在 5min 内实现分离。通过与 2,3-萘二羧酸醛（NDA）进行柱前衍生化，实现了对 ALEN 的 FL 检测。在 7-200ng/mL ALEN 范围内，FL 强度与分析物浓度之间呈线性相关（r=0.9981，n=6）。该 CE-FL 方法已应用于人尿和血浆样品中 ALEN 的分析。为了消除干扰基质成分，采用基于磁性 Fe(3)O(4)@Al(2)O(3)纳米粒子的固相萃取（SPE）在 CE-FL 分析前对生物流体进行净化。ALEN 在尿和血浆中的线性范围分别为 5-100ng/mL（r=0.9982，n=7）和 5-70ng/mL（r=0.9954，n=7）。在尿液和血浆样品中，ALEN 的 LOD 和 LOQ 分别为 1.5 和 5ng/mL。包括样品预处理和 CE 分离在内的总分析时间小于 1.5h。
