Ahmad Abdel Kader S, Kawy M Abdel, Nebsen M
Faculty of Pharmacy, Analytical Chemistry Department, Cairo University, Kasr El-Aini Street, 11562 Cario, Egypt.
J Pharm Biomed Anal. 2002 Oct 15;30(3):479-89. doi: 10.1016/s0731-7085(02)00132-2.
Three methods are presented for the determination of Nicergoline in presence of its hydrolysis-induced degradation product. The first method was based on measurement of the first derivative of ratio spectra amplitude of Nicergoline at 291 nm. The second method was based on separation of Nicergoline from its degradation product followed by densitometric measurement of the spots at 287 nm. The separation was carried out on HPTLC silica gel F(254) plates, using methanol-ethyl acetate-glacial acetic acid (5:7:3, v/v/v) as mobile phase. The third method was based on high performance liquid chromatographic (HPLC) separation and determination of Nicergoline from its degradation product on a reversed phase, nucloesil C(18) column using a mobile phase of methanol-water-glacial acetic acid (80:20:0.1, v/v/v) with UV detection at 280 nm. Chlorpromazine hydrochloride was used as internal standard. Laboratory prepared mixtures containing different percentages of the degradation product were analysed by the proposed methods and satisfactory results were obtained. These methods have been successfully applied to the analysis of Nicergoline in Sermion tablets. The validities of these methods were ascertained by applying standard addition technique, the mean percentage recovery +/- R.S.D.% was found to be 99.47 +/- 0.752, 100.01 +/- 0.940, 99.75 +/- 0.740 for the first derivative of ratio spectra method, the HPTLC method and the HPLC method, respectively. The proposed methods were statistically compared with the manufacturer's HPLC method of analysis of Nicergoline and no significant difference was found with respect to both precision and accuracy. They have the advantage of being stability indicating. Therefore, they can be used for routine analysis of the drug in quality control laboratories.
本文介绍了三种在尼麦角林存在水解诱导降解产物的情况下测定尼麦角林的方法。第一种方法基于测量尼麦角林在291nm处的比率光谱振幅的一阶导数。第二种方法是先将尼麦角林与其降解产物分离，然后对287nm处的斑点进行光密度测定。分离在HPTLC硅胶F(254)板上进行，以甲醇 - 乙酸乙酯 - 冰醋酸(5:7:3, v/v/v)为流动相。第三种方法基于高效液相色谱(HPLC)分离，并在反相核硅C(18)柱上测定尼麦角林及其降解产物，流动相为甲醇 - 水 - 冰醋酸(80:20:0.1, v/v/v)，在280nm处进行紫外检测。盐酸氯丙嗪用作内标。用所提出的方法分析了实验室制备的含有不同百分比降解产物的混合物，并获得了满意的结果。这些方法已成功应用于Sermion片剂中尼麦角林的分析。通过标准加入技术确定了这些方法的有效性，比率光谱一阶导数法、HPTLC法和HPLC法的平均回收率±相对标准偏差(R.S.D.%)分别为99.47±0.752、100.01±0.940、99.75±0.740。将所提出的方法与制造商分析尼麦角林的HPLC方法进行了统计学比较，在精密度和准确度方面均未发现显著差异。它们具有指示稳定性的优点。因此，可用于质量控制实验室对该药物的常规分析。
