ABSTRACT
Despite several studies on the Ajuga L. genus, the chemical composition of Ajuga pyramidalis, an alpine endemic species, is still largely unknown. The purpose of this study was to therefore deeper describe it, particularly from the phytochemistry and bioactivity perspectives. In that respect, A. pyramidalis was investigated and 95% of the extracted mass of the plant was characterized by chromatography and mass spectrometry. Apart from the already determined chemical compounds, namely, harpagide and 8-O-acetylharpagide, two iridoids, and neoajugapyrin A, a neo-clerodane diterpene, and three polyphenols (echinacoside, verbascoside and teupoloside) were identified for the first time in A. pyramidalis. Incidentally, the first RX structure of a harpagoside derivative is also described in this paper. The extracts and isolated compounds were then evaluated for various biochemical or biological activities; notably a targeted action on the renewal of the epidermis was highlighted with potential applications in the cosmetic field for anti-aging.
ABSTRACT
The active component extraction from plants is the first crucial step in natural product research. For non-targeted extraction with an objective to isolate and characterize as many compounds as possible, the most classical technique, and the simplest to implement, is the Soxhlet extraction; however, it does not allow retrieving all the compounds from the plant (when it does not additionally cause artifacts during long heating process). The second most used technique is the extraction by successive macerations using solvents of increasing polarity. While this method is frequently used, few studies are available to rationalize and optimize it. Furthermore, this extraction technique requires some enhancement mainly for efficiency, environmental and time constraint reasons. Here, we present an innovative method of successive macerations using a mixture of solvents with the aim of simultaneously improving the yield, the partition of the compounds between the different phases and reducing the volume of extraction solvents. Triphasic systems were prepared by mixing five solvents (n-heptane, ethyl acetate, acetonitrile, butan-1-ol, water) in various proportions. To validate this method, the most efficient triphasic system was subsequently used to perform three successive macerations with a polarity gradient on a model plant before being extended to several alpine plants. Our results showed an overall good yield compared to conventional maceration techniques, while improving phase partition and reducing extraction time and volume of solvents.
Subject(s)
Biological Products/isolation & purification , Chemical Fractionation/methods , Phytochemicals/isolation & purification , Solvents , Biological Products/chemistry , Phytochemicals/chemistryABSTRACT
A new strategy was developed to elucidate and quantify 56 (69 analytes including isomers) suspected chemically defined fragrance allergens in perfumes that were recently targeted by the Scientific Committee on Consumer Safety (SCCS). Samples were analyzed with a two-dimensional gas chromatography-quadrupole mass spectrometry system (GC-GC-MS). Method performance was evaluated by the accuracy profile approach to determine uncertainties around the regulation limit of 10mg/kg. This strategy was finally applied to 62 commercialized perfumes, analyzed in the routine workflow. Depending on the matrix, an acceptable result was obtained for 88-100% of the target analytes, which means that results were accurately defined under or above 10mg/kg. This method saves considerable time for complete analysis and could be adopted for routine analysis due to its ruggedness and cost effectiveness.
