El-Enany Nahed
Mansoura University, Faculty of Pharmacy, Department of Analytical Chemistry, Mansoura 35516, Egypt.
J AOAC Int. 2007 Jul-Aug;90(4):948-56.
Two simple, sensitive, and specific spectrofluorometric procedures have been developed for the determination of labetalol (LBT) in pharmaceuticals and biological fluids. LBT was found to react with Al3+, both in acetate buffer of pH 4.5 (Procedure I) and borate buffer of pH 8.0 (Procedure II), to produce highly fluorescent stable complexes. The fluorescence intensity could be enhanced by the addition of sodium dodecyl sulfate, resulting in 3.5- and 2.7-fold increases in the fluorescence intensity for Procedures I and II, respectively. In both procedures, the fluorescence intensity was measured at 408 nm after excitation at 320 nm. The different experimental parameters affecting the development and stability of the fluorescent products were carefully studied and optimized. The fluorescence intensity-concentration plots were rectilinear over the range of 0.02-0.1 and 0.01-0.05 microg/mL with a detection limit of 0.003 and 0.001 microg/mL for Procedures I and II, respectively. The proposed method was successfully applied to commercial tablets containing LBT. The results were in good agreement with those obtained using a reference spectrofluorometric method. Furthermore, the method was applied for the determination of LBT in spiked human plasma, and the recovery (n = 4) was 93.30 +/- 2.62%. A proposal of the reaction pathway was postulated for Procedures I and II, respectively.
已开发出两种简单、灵敏且特异的荧光分光光度法,用于测定药物制剂和生物流体中的拉贝洛尔(LBT)。发现LBT在pH 4.5的醋酸盐缓冲液(方法I)和pH 8.0的硼酸盐缓冲液(方法II)中均能与Al3+反应,生成高荧光稳定络合物。加入十二烷基硫酸钠可增强荧光强度,方法I和方法II的荧光强度分别增加3.5倍和2.7倍。在两种方法中,均在320nm激发后于408nm处测量荧光强度。仔细研究并优化了影响荧光产物形成和稳定性的不同实验参数。方法I和方法II的荧光强度-浓度曲线在0.02 - 0.1和0.01 - 0.05μg/mL范围内呈线性,检测限分别为0.003和0.001μg/mL。所提出的方法成功应用于含LBT的市售片剂。结果与采用参考荧光分光光度法获得的结果良好吻合。此外,该方法还应用于加标人血浆中LBT的测定,回收率(n = 4)为93.30 +/- 2.62%。分别推测了方法I和方法II的反应途径。