Shirkhedkar Atul A, Bugdane Prasad M, Surana Sanjay J
R.C. Patel College of Pharmacy, Shirpur Dist: Dhule, (M.S.) 425 405 India.
J Chromatogr Sci. 2010 Feb;48(2):109-13. doi: 10.1093/chromsci/48.2.109.
A simple, selective, precise, and stability-indicating high-performance thin-layer chromatographic (HPTLC) method for densitometric determination of nebivolol hydrochloride both as a bulk drug and in formulation was developed and validated as per the international conference on harmonization guidelines (ICH). The method employed TLC aluminium plates precoated with silica gel 60F254 as the stationary phase. The solvent system consisted of toluene-methanol-triethylamine (3.8:1.2:0.2 v/v/v). Densitometry analysis of nebivolol hydrochloride was carried out in the absorbance mode at 281 nm. The system was found to give compact spot for nebivolol hydrochloride (R(f) value of 0.33 +/- 0.02). The linear regression analysis data for the calibration plots showed good relationship with r(2)= 0.9994 +/- 0.0002 in the concentration range 500-3000 ng/spot. The mean value +/- SD of slope and intercept were 3.761 +/- 0.017 and 127.39 +/- 19.53 with respect to peak area. The limits of detection (LOD) and limit of quantitation (LOQ) were 63.10 ng/spot and 191.23 ng/ spot, respectively. Nebivolol hydrochloride was subjected to acid and alkali hydrolysis, oxidation, thermal degradation, and photodegradation. All the peaks of degradation products were well-resolved from the standard drug with significantly different R(f) values. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of said drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of nebivolol hydrochloride in the bulk and pharmaceutical dosage form.
根据国际协调会议指南（ICH），开发并验证了一种简单、选择性强、精确且具有稳定性指示功能的高效薄层色谱（HPTLC）方法，用于密度测定盐酸奈必洛尔原料药及其制剂。该方法采用预涂硅胶60F254的TLC铝板作为固定相。溶剂系统由甲苯 - 甲醇 - 三乙胺（3.8:1.2:0.2 v/v/v）组成。盐酸奈必洛尔的密度测定分析在281 nm吸光度模式下进行。该系统对盐酸奈必洛尔产生紧密斑点（R(f)值为0.33±0.02）。校准曲线的线性回归分析数据显示在500 - 3000 ng/斑点的浓度范围内具有良好的关系，r(2)= 0.9994±0.0002。相对于峰面积，斜率和截距的平均值±标准差分别为3.761±0.017和127.39±19.53。检测限（LOD）和定量限（LOQ）分别为63.10 ng/斑点和191.23 ng/斑点。盐酸奈必洛尔进行了酸、碱水解、氧化、热降解和光降解。所有降解产物的峰与标准药物峰得到了很好的分离，R(f)值有显著差异。统计分析证明该方法对于所述药物的估计是可重复、选择性和准确的。所提出的HPTLC方法可用于盐酸奈必洛尔原料药和药物剂型的鉴别和定量测定。
