Dhalwal Kamlesh, Shinde Vaibhav M, Namdeo Ajay G, Mahadik Kakasaheb R, Kadam Shivajirao S
Poona College of Pharmacy, Bharati Vidyapeeth Deemed University, Erandwane, Pune- 411 038, Maharashtra, India.
J Chromatogr Sci. 2007 Nov-Dec;45(10):706-9. doi: 10.1093/chromsci/45.10.706.
A simple, sensitive, and specific thin-layer chromatography densitometric method has been developed for the simultaneous quantitation of strychnine and brucine. These two marker compounds are quantitated in the seeds of Strychnos nux-vomica, Strychnos ignatii, and its formulations. The method involves densitometric evaluation of strychnine and brucine after resolving it by high-performance TLC on silica gel plate with toluene-ethyl acetate-diethyl amine-methanol (7:2:1:0.3 v/v) as the mobile phase. The method is validated for precision (interday and intraday), repeatability, and accuracy. The relationship between the concentration of standard solutions and the peak response is linear within the concentration range of 160 to 480 ng/spot for strychnine and 80 to 480 ng/spot for brucine. Instrumental precision is found to be 0.54 and 0.78 (% CV), and repeatability of the method is 1.01 and 1.06 (% CV) for strychnine and brucine, respectively. Accuracy of the method is checked by recovery study conducted at three different levels and the average percentage recovery is found to be 99.13% for strychnine and 100.16% for brucine. The proposed HPTLC method for the simultaneous quantitation of strychnine and brucine is found to be simple, precise, specific, sensitive, and accurate, and it can be used for routine quality control of raw material of Strychnos spp. It also can be applied in quantitating any of these marker compounds in other formulations.
已开发出一种简单、灵敏且特异的薄层色谱密度测定法，用于同时定量士的宁和马钱子碱。这两种标记化合物在马钱子、吕宋豆及其制剂的种子中进行定量。该方法包括在硅胶板上以甲苯 - 乙酸乙酯 - 二乙胺 - 甲醇（7:2:1:0.3 v/v）为流动相，通过高效薄层色谱分离后，对士的宁和马钱子碱进行密度测定评估。该方法在精密度（日间和日内）、重复性和准确性方面得到了验证。士的宁标准溶液浓度在160至480 ng/斑点范围内，马钱子碱标准溶液浓度在80至480 ng/斑点范围内，标准溶液浓度与峰响应之间的关系呈线性。仪器精密度分别为0.54和0.78（%CV），该方法对士的宁和马钱子碱的重复性分别为1.01和1.06（%CV）。通过在三个不同水平进行回收率研究来检查该方法的准确性，发现士的宁的平均回收率为99.13%，马钱子碱的平均回收率为100.16%。所提出的同时定量士的宁和马钱子碱的高效薄层色谱法简单、精确、特异、灵敏且准确，可用于马钱子属植物原料的常规质量控制。它也可应用于其他制剂中这些标记化合物的定量分析。
