|Avula, Bharathi -|
|Shukla, Yatin -|
|Wang, Yan-Hong -|
|Khan, Ikhas -|
Submitted to: Official Methods of Analysis of AOAC International
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: January 6, 2011
Publication Date: September 1, 2011
Citation: Avula, B., Shukla, Y.J., Wang, Y., Khan, I.A. 2011. Chemical fingerprint analysis and quantitative determination of pregnanes from aerial parts of caralluma species using HPLC-UV and identification by LC-ESI-TOF. Official Methods of Analysis of AOAC International. 94(5):1383-1390. Interpretive Summary: A simple, precise HPLC-UV method was developed for the determination of five compounds (boucerin, caraumbelloside I, caraumbelloside III, caraumbelloside II and caraumbellogenin). The developed method was applied for the chemical fingerprint analysis of Caralluma species. The identification of these compounds was confirmed by a more sensitive LC-MS-TOF technique. Analytical method development becomes crucial for product validity and safety.
Technical Abstract: A HPLC method is developed for the quantitative determination of five pregnane derivatives from aerial parts of Caralluma species and dietary supplements. The method is validated for linearity, repeatability, limits of detection (LOD) and limits of quantification (LOQ). The limits of detection and limits of quantification of five pregnane compounds are found to be in the range from 1-5 µg/mL and 3-15 µg/mL, respectively by HPLC with a detection using PDA detector. This method is applied to the chemical fingerprint identification of three plant materials of Caralluma species (C. fimbriata, C. umbellata and C. attentuata) and seven dietary supplements claiming to contain C. fimbriata. LC-mass spectrometry coupled with electrospray ionization (ESI) interface method is described for the identification of compounds and involved the use of [M+Na]+ ions in the positive ion mode with extracted ion chromatogram (XIC).