H.E.J. Research Institute of Chemistry, International Centers for Chemical and Biological Sciences (ICCBS), University of Karachi, Karachi 75270, Pakistan.
J Pharm Biomed Anal. 2011 Sep 10;56(2):240-5. doi: 10.1016/j.jpba.2011.05.021. Epub 2011 May 20.
A high performance thin-layer chromatographic (HPTLC) method for the simultaneous determination of the hypolipidemic agents, E- and Z-isomers of guggulsterone in Commiphora mukul resin, guggulipid (ethyl acetate extract of resin), and its pharmaceutical formulation, was developed. The developed system was efficient enough to separate both isomers from their conger, 17,20-dihydroguggulsterone. HPTLC glass plates, pre-coated with silica gel 60F-254, were used as a stationary phase. The mobile phase consisted of toluene:acetone (9.3:0.7, v/v) which gave well resolved spots for E- and Z-guggulsterones (R(f): 0.52±0.01, and 0.67±0.01, respectively) following double development of chromatoplate with the same mobile phase under unsaturated conditions. The analyte stability towards the developed chromatographic procedure was also investigated by two-dimensional (2D) HPTLC analysis. 17,20-Dihydroguggulsterone (3) was identified by the electrospray ionization quadrupole time-of-flight tandem mass spectrometry (ESI-QTOF-MS/MS) analysis.
建立了一种高效薄层色谱(HPTLC)法,用于同时测定 Commiphora mukul 树脂中的降脂剂 E-和 Z-型古卡二醇、古卡脂(树脂的乙酸乙酯提取物)及其药物制剂中的两种异构体。该方法的分离效率足以将两种异构体与其同源物 17,20-二氢古卡二醇分离开来。采用涂有硅胶 60F-254 的 HPTLC 玻璃板作为固定相。流动相由甲苯:丙酮(9.3:0.7,v/v)组成,在不饱和条件下,采用相同的流动相进行两次展开后,可得到 E-和 Z-古卡二醇的分离度良好的斑点(R(f):分别为 0.52±0.01 和 0.67±0.01)。还通过二维(2D)HPTLC 分析研究了分析物对开发的色谱程序的稳定性。通过电喷雾电离四极杆飞行时间串联质谱(ESI-QTOF-MS/MS)分析鉴定了 17,20-二氢古卡二醇(3)。