Journal
CHROMATOGRAPHIA
Volume 70, Issue 11-12, Pages 1613-1619Publisher
SPRINGER HEIDELBERG
DOI: 10.1365/s10337-009-1347-x
Keywords
Ultra performance liquid chromatography; Tandem mass spectrometry; Method validation; E- and Z-guggulsterone; Commiphora wightii
Funding
- Waters India Pvt. Ltd, Bangalore, India
- Department of Agriculture, Government of Jharkhand
- Department of Biotechnology, Government of India [102/IFD/SAN/1192/2004-05]
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A fast and simple method for simultaneous detection and quantification of the medicinally important E- and Z-guggulsterone from raw oleogum-resin of Commiphora wightii by UPLC was developed. Both E- and Z-guggulsterone were extracted from naturally occurring resin samples using ethyl acetate and methanol. Chromatographic separation of the analytes and their respective standards were performed on an Acquity UPLC BEH C-18 column followed by UV as well as a triple quadrupole detector in positive ionization mode. A linear gradient elution profile followed; mobile phase consisted of acetonitrile and 2 mM ammonium acetate in water. The method was validated over a range of 6.25 to 100 ng mL(-1) for both the guggulsterones. The calibration curves were linear with correlation coefficients of 0.9998 for E-guggulsterone and 0.9999 for Z-guggulsterone. The LOD and LOQ were 1.65 and 5.02 ng mL(-1) for E-guggulsterone and 2.57 and 7.79 ng mL(-1) for Z-guggulsterone respectively. The average recovery of E-guggulsterone (104.63%) and Z-guggulsterone (104.33%) achieved from spiked samples were consistent and reproducible. The intra- and inter-day assay precision of the analytes over the entire concentration range was less than 2%. The developed method required only 6 min to complete a run including 1 min to equilibrate the system and hence suitable for high throughput applications. Efficiency, reliability and accuracy of the developed method were evaluated by analyzing resin sample from different C. wightii populations. The result of this study offers improvement in terms of speed and sensitivity as compared to previously reported methods.
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