Walash Mohamed I, Belal Fathalla, El-Enany Nahed, Abdelal Amina
University of Mansoura, Faculty of Pharmacy, Department of Analytical Chemistry, 35516, Mansoura, Egypt.
J AOAC Int. 2008 Mar-Apr;91(2):349-59.
A rapid, simple, and highly sensitive second-derivative synchronous fluorometric method has been developed for the simultaneous analysis of binary mixtures of cinnarizine (CN) and nicergoline (NIC). The method is based upon measurement of the native fluorescence of these drugs at constant wavelength difference (Deltalambda) = 80 nm in aqueous methanol (50%, v/v). The different experimental parameters affecting the native fluorescence of the studied drugs were carefully studied and optimized. The fluorescence-concentration plots were rectilinear over the range of 0.025-1.5 and 0.25-5.5 microg/mL for CN and NIC, respectively, with lower detection limits of 0.58 and 0.82 ng/mL and quantitation limits of 1.93 and 2.73 ng/mL for CN and NIC, respectively. The proposed method was successfully applied for the determination of the studied compounds in synthetic mixtures and in commercial tablets. The results obtained were in good agreement with those obtained with reference methods. The high sensitivity attained by the proposed method allowed the determination of CN in real and spiked human plasma. The mean recovery in the case of spiked human plasma [number of trials (n) = 3] was 102.82 +/- 2.17%, while that in real human plasma (n = 3) was 105.25 +/- 2.05.
已开发出一种快速、简单且高度灵敏的二阶导数同步荧光法，用于同时分析桂利嗪（CN）和尼麦角林（NIC）的二元混合物。该方法基于在水 - 甲醇（50%，v/v）中，在恒定波长差（Δλ） = 80 nm下测量这些药物的天然荧光。仔细研究并优化了影响所研究药物天然荧光的不同实验参数。对于CN和NIC，荧光 - 浓度曲线在0.025 - 1.5和0.25 - 5.5 μg/mL范围内分别呈线性，CN和NIC的检测限分别为0.58和0.82 ng/mL，定量限分别为1.93和2.73 ng/mL。所提出的方法成功应用于合成混合物和市售片剂中所研究化合物的测定。获得的结果与参考方法得到的结果高度一致。所提出方法达到的高灵敏度使得能够测定实际和加标人血浆中的CN。加标人血浆[试验次数（n） = 3]的平均回收率为102.82 +/- 2.17%，而实际人血浆（n = 3）中的平均回收率为105.25 +/- 2.05。
