Development of a gas chromatography–mass spectrometry method to monitor in a single run, mono- to triterpenoid compounds distribution in resinous plant materials
Autor: | Agnes Chartier, Zaineb Jemmali, Claire Elfakir |
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Přispěvatelé: | Institut de Chimie Organique et Analytique (ICOA), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université d'Orléans (UO)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Institut National de la Santé et de la Recherche Médicale (INSERM), Centre National de la Recherche Scientifique (CNRS)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université d'Orléans (UO)-Institut de Chimie du CNRS (INC) |
Jazyk: | angličtina |
Rok vydání: | 2016 |
Předmět: |
0106 biological sciences
Trimethylsilyl Carboxylic acid Carboxylic Acids Mass spectrometry 01 natural sciences Biochemistry Chemistry Techniques Analytical Gas Chromatography-Mass Spectrometry Analytical Chemistry chemistry.chemical_compound Triterpene [CHIM]Chemical Sciences Derivatization ComputingMilieux_MISCELLANEOUS chemistry.chemical_classification Principal Component Analysis Chromatography Terpenes 010401 analytical chemistry Organic Chemistry General Medicine BSTFA 0104 chemical sciences chemistry Gas chromatography Gas chromatography–mass spectrometry Resins Plant 010606 plant biology & botany |
Zdroj: | Journal of Chromatography A Journal of Chromatography A, 2016, 1443, pp.241-253. ⟨10.1016/j.chroma.2016.03.031⟩ Journal of Chromatography A, Elsevier, 2016, 1443, pp.241-253. ⟨10.1016/j.chroma.2016.03.031⟩ |
ISSN: | 0021-9673 1873-3778 |
DOI: | 10.1016/j.chroma.2016.03.031⟩ |
Popis: | 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. |
Databáze: | OpenAIRE |
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