Al-Kindy Salma M Z, Al-Harasi Zakiya, Suliman Fakhr Eldin O, Al-Hamadi Abdalla, Pillay Avin
Department of Chemistry, Sultan Qaboos University, College of Science, Box 36, Al-Khod 123, Muscat, Sultanate of Oman.
J Fluoresc. 2009 Mar;19(2):249-55. doi: 10.1007/s10895-008-0410-6. Epub 2008 Sep 5.
This paper explores an ultra-sensitive luminescence method for the determination of Ketoprofen (KP) in pharmaceutical formulations. The technique is indirect and exploits the luminescence enhancement of terbium (Tb(3+)) by complexation with KP (Tb(3+)-KP), which was monitored at respective excitation and emission wavelengths of lambda(ex) = 258 nm and lambda(em) = 549 nm. The effect of varying the Tb(3+) concentration and using multiple solvents was examined to determine optimal experimental conditions. Maximum sensitization was accomplished in the presence of methanol where the most favourable condition for the formation of the complex was recorded at a level of 1.0 x 10(-5) M of Tb(3+). Under these optimum experimental conditions, linear calibration curve was obtained in the range of 2.8 x 10(-7)-3.1 x 10(-6) M with a detection limit of 8.7 x 10(-8) M. The technique was validated with 'working' reference standards and produced relative standard deviations < 2% indicating that the reproducibility was highly acceptable. The proposed method was successfully applied to assays of KP in pharmaceutical formulations with average recoveries of 92-98%. The results were found to be in good agreement with those obtained by HPLC. The method is highly suited for general applications of this nature.
本文探索了一种用于测定药物制剂中酮洛芬(KP)的超灵敏发光方法。该技术是间接的,利用了铽(Tb(3+))与KP络合(Tb(3+)-KP)时发光增强的现象,在激发波长λ(ex)=258 nm和发射波长λ(em)=549 nm处进行监测。研究了改变Tb(3+)浓度和使用多种溶剂的影响,以确定最佳实验条件。在甲醇存在下实现了最大增敏效果,记录到形成络合物的最有利条件是Tb(3+)浓度为1.0×10(-5) M。在这些最佳实验条件下,获得了2.8×10(-7)-3.1×10(-6) M范围内的线性校准曲线,检测限为8.7×10(-8) M。该技术用“工作”参考标准进行了验证,相对标准偏差<2%,表明重现性非常好。所提出的方法成功应用于药物制剂中KP的测定,平均回收率为92-98%。结果与通过高效液相色谱法获得的结果高度一致。该方法非常适合此类一般应用。