Chopra Shruti, Ahmad Farhan J, Khar Roop K, Motwani Sanjay K, Mahdi Saiqa, Iqbal Zeenat, Talegaonkar Sushma
Department of Pharmaceutics, Faculty of Pharmacy, Jamia Hamdard, Hamdard Nagar, New Delhi 110062, India.
Anal Chim Acta. 2006 Sep 1;577(1):46-51. doi: 10.1016/j.aca.2006.06.034. Epub 2006 Jun 21.
A new, simple, sensitive, selective, precise and robust high-performance thin-layer chromatographic (HPTLC) method for analysis of trigonelline was developed and validated for the determination of trigonelline in herbal extracts and in pharmaceutical dosage forms. Analysis of trigonelline was performed on TLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase. Linear ascending development was carried out in twin trough glass chamber saturated with mobile phase consisting of n-propanol-methanol-water (4:1:4, v/v/v) at room temperature (25+/-2 degrees C). Camag TLC scanner III was used for spectrodensitometric scanning and analysis in absorbance mode at 269 nm. The system was found to give compact spots for trigonelline (R(f) value of 0.46+/-0.02). The linear regression analysis data for the calibration plots showed good linear relationship with r2=0.9991+/-0.0002 in the concentration range 100-1200 ng spot(-1) with respect to peak area. According to the International Conference on Harmonization (ICH) guidelines the method was validated for precision, recovery, robustness and ruggedness. The limits of detection and quantification were determined. The trigonelline content of herbal extracts quantified and estimated from the formulation was found to be well within limits (+/-5% of the labeled content of the formulations). Statistical analysis of the data showed that the method is reproducible and selective for the estimation of trigonelline.
开发了一种用于分析胡芦巴碱的新型、简单、灵敏、选择性好、精确且稳健的高效薄层色谱（HPTLC）方法，并对其在草药提取物和药物剂型中胡芦巴碱的测定进行了验证。以预涂硅胶60F - 254的TLC铝板为固定相进行胡芦巴碱分析。在室温（25±2℃）下，在充满由正丙醇 - 甲醇 - 水（4:1:4，v/v/v）组成的流动相的双槽玻璃室中进行线性上行展开。使用Camag TLC扫描仪III在269nm吸光度模式下进行光密度扫描和分析。该系统对胡芦巴碱给出致密斑点（R(f)值为0.46±0.02）。校准曲线的线性回归分析数据显示，在100 - 1200ng斑点⁻¹浓度范围内，相对于峰面积具有良好的线性关系，r² = 0.9991±0.0002。根据国际协调会议（ICH）指南，对该方法的精密度、回收率、稳健性和耐用性进行了验证。测定了检测限和定量限。从制剂中定量和估算的草药提取物中胡芦巴碱含量发现完全在限度内（制剂标示含量的±5%）。数据的统计分析表明，该方法对于胡芦巴碱的估算具有可重复性和选择性。
