Quantitative Determination of thymoquinone in Nigella Sativa and its nano formulation using validated stability indicating HPTLC densiometric method

M. Taleuzzaman, S. Imam, S. Gilani
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引用次数: 9

Abstract

An accurate and stability indicating high-performance thin layer chromatographic method (HPTLC) was developed and validated for the quantification of thymoquinone (TQ) as per the ICH guidelines. The analysis was carried out on the aluminum plate using n-hexane: ethyl acetate: methanol (7:2:1 v/v/v) as the mobile phase and the densitometric determination was carried out by TLC scanner (CAMAG) at 254 nm. The developed method was validated for different parameters like linearity, precision, recovery, robustness, and stressed stability study. The developed analytical method was found to be linear in the concentration range of 75-500 ng band -1 with regression value closer to unity (r 2 = 0.997). The developed system was found to give compact spots for thymoquinone (R f 0.77) with the limit of detection and limit of quantification (18 and 54 ng band -1 ) respectively. Further, the study showed accuracy, precision and repeatability were all within the required limits. The stress degradation study of TQ showed well separated degraded peak from the pure thymoquinone. The mean recoveries measured at three concentrations were more than 95% with RSD ≤ 3%. The method has been successfully applied in the analysis and routine quality control of herbal material and formulations containing TQ. Taleuzzaman et al., International Current Pharmaceutical Journal, September 2017, 6(10): 53-60 http://www.icpjonline.com/documents/Vol6Issue10/01.pdf
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高效液相色谱法定量测定黑草中百里醌及其纳米制剂的含量
建立了一种准确、稳定的高效薄层色谱(HPTLC)定量百里醌(TQ)方法,并根据ICH指南进行了验证。以正己烷:乙酸乙酯:甲醇(7:2:1 v/v/v)为流动相,在铝板上进行分析,采用薄层扫描(CAMAG)在254 nm处进行密度测定。对该方法进行了线性度、精密度、回收率、鲁棒性和应力稳定性等参数的验证。结果表明,该方法在75 ~ 500 ng波段-1的浓度范围内线性良好,回归值接近1 (r 2 = 0.997)。结果表明,该体系对百里醌的检测下限和定量下限分别为18和54 ng波段-1,斑点紧凑(R = 0.77)。此外,研究表明,准确度、精密度和重复性均在要求的范围内。对TQ的应激降解研究表明,其降解峰与纯百里醌分离良好。3种浓度下的平均加样回收率均大于95%,RSD≤3%。该方法已成功应用于含TQ的中草药及制剂的分析和常规质量控制。Taleuzzaman等,国际药学杂志,2017,6(10):53-60 http://www.icpjonline.com/documents/Vol6Issue10/01.pdf
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