title: Development of a gas chromatography-mass spectrometry method to monitor in a single run, mono- to triterpenoid compounds distribution in resinous plant materials.
abstract: A new procedure based on gas chromatography coupled to mass spectrometry (GC-MS) was developed for the simultaneous determination of mono- to triterpenoid compounds in resinous materials. Given the difference of volatility and polarity of the studied compounds some critical steps in this methodology had to be identified and investigated. The recovery of volatile compounds after sample extraction was studied. A recovery range from 30% to 100% from the more volatile monoterpene to the least one was observed. Then the mandatory derivatization step for the analysis of pentacyclic triterpenes bearing hydroxyl and carboxyl groups was optimized. Results showed that derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and trimethylchlorosilane (TMCS) in pyridine (22:13:65 v/v/v) for 2h at 30 °C was the most efficient method of derivatizing all the hydroxyl and carboxylic acid groups contained in the triterpene structures. After choosing the best injection parameters for these compounds, the selectivity of the GC column towards the separation of these terpenoids was investigated using statistical tools (principal component analysis and desirability functions). A separation with a good resolution was achieved on an HP-5ms column using a programmed temperature vaporizing injector (PTV). The method was pre-validated in terms of detection limits (LOD from 100 μg L(-1) to 200 μg L(-1) depending on the compound), linearity and repeatability using seven compounds representative of mono- and triterpenoid classes. An exhaustive characterization of various types of resins (di-, triterpenic and oleo-gum resins) was achieved.
authors.affiliation: Univ-Orleans, CNRS, ICOA, UMR 7311, F-45067 Orléans, France.
authors.forename: Zaineb
authors.initials: Z
authors.lastname: Jemmali
authors.affiliation: Univ-Orleans, CNRS, ICOA, UMR 7311, F-45067 Orléans, France. Electronic address: agnes.chartier@univ-orleans.fr.
authors.forename: Agnes
authors.initials: A
authors.lastname: Chartier
authors.affiliation: Univ-Orleans, CNRS, ICOA, UMR 7311, F-45067 Orléans, France.
authors.forename: Claire
authors.initials: C
authors.lastname: Elfakir
mesh_terms: D002264:Carboxylic Acids / Q000737:chemistry; D002623:Chemistry Techniques, Analytical; D008401:Gas Chromatography-Mass Spectrometry; D025341:Principal Component Analysis; D012116:Resins, Plant / Q000032:analysis* / Q000737:chemistry*; D013729:Terpenes / Q000032:analysis* / Q000737:chemistry
chemical_list: D002264:Carboxylic Acids; D012116:Resins, Plant; D013729:Terpenes
keywords: Boswellia serrata; Commiphora wildii; Copal; GC/MS; Oleo-gum resins; Pistacia lentiscus; Terpenoids