Dinç Erdal, Kaya Süha, Doganay Tanver, Baleanu Dumitru
Department of Analytical Chemistry, Faculty of Pharmacy, Ankara University, 06100 Tandoğan, Ankara, Turkey.
J Pharm Biomed Anal. 2007 Aug 15;44(4):991-5. doi: 10.1016/j.jpba.2007.03.027. Epub 2007 Mar 30.
Simultaneous analyses and dissolution tests of levodopa-benserazide tablets were carried out by continuous wavelet transform (CWT) and classic derivative spectrophotometry (DS) without using any chemical separation step. The developed two spectrophotometric resolutions are based on the transformation of the original UV spectra. The original absorption spectra of levodopa and benserazide in the concentration range of 1-80 microg/mL and 5-240 microg/mL in USP simulated gastric juice were registered in the spectral range of 250-310 nm, respectively. Various wavelet families and different spectrophotometric derivative orders were tested to find the optimal signal processing for obtaining desirable calibration graphs and reliable determinations of the investigated drugs. Under the optimized conditions of the methods, symlets wavelet family using a=128 with sixth order (SYM6-CWT) and the first derivative transform with Deltalambda=10nm were identified as optimal signal processing methods for the determinations and dissolution tests. The calibration functions for each drug were obtained by measuring the values of the CWT and derivative amplitudes. The validation of the developed methods was confirmed by analyzing various synthetic mixtures of the investigated drugs. Mean recovery values were found between 99.1% and 104.7% for DS and 100% and 102.9% for CWT, respectively for determination of BEN and LEV in synthetic mixtures. Each developed approaches were successfully applied to the simultaneous determination and dissolution test of levodopa and benserazide in their commercial tablets and a good agreement was observed.
采用连续小波变换(CWT)和经典导数分光光度法(DS)对左旋多巴-苄丝肼片进行同步分析和溶出度试验,无需任何化学分离步骤。所开发的两种分光光度法分辨率基于原始紫外光谱的变换。在USP模拟胃液中,左旋多巴和苄丝肼在1 - 80μg/mL和5 - 240μg/mL浓度范围内的原始吸收光谱分别在250 - 310nm光谱范围内进行记录。测试了各种小波族和不同的分光光度导数阶数,以找到最佳信号处理方法,从而获得理想的校准曲线并可靠地测定所研究的药物。在方法的优化条件下,使用a = 128的symlets小波族和六阶(SYM6 - CWT)以及Δλ = 10nm的一阶导数变换被确定为测定和溶出度试验的最佳信号处理方法。通过测量CWT值和导数幅度获得每种药物的校准函数。通过分析所研究药物的各种合成混合物,证实了所开发方法的有效性。在合成混合物中测定BEN和LEV时,DS的平均回收率分别在99.1%至104.7%之间,CWT的平均回收率在100%至102.9%之间。所开发的每种方法都成功应用于左旋多巴和苄丝肼市售片剂的同时测定和溶出度试验,并观察到良好的一致性。