NMR, HS‐SPME‐GC/MS, and HPLC/MSⁿ Analyses of Phytoconstituents and Aroma Profile of Rosmarinus eriocalyx

Abstract

In this work, a comprehensive study on the chemical constituents of the aerial parts of Rosmarinus eriocalyx (Lamiaceae), an aromatic shrub traditionally consumed as a food and herbal remedy in Algeria, is presented. The aroma profile was analysed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC/MS), whereas the crude extract constituents were analyzed by H-NMR and by high performance liquid chromatography coupled with mass spectrometry (HPLC/MS ). Thirty-nine volatile compounds, most of them being monoterpenes, have been identified, with camphor, camphene, and α-pinene as the most abundant constituents. H-NMR analysis revealed the presence of phenolic compounds and betulinic acid while HPLC/MS allowed the identification of glycosilated and aglyconic flavonoids as well as phenylpropanoid derivatives. Some of these constituents, namely as betulinic acid, rosmanol, and cirsimaritin were reported for the first time in R. eriocalyx.

Characterization of Polyphenols and Volatile Compounds from Understudied Algerian Pallenis spinosa by HS-SPME-GC-MS, NMR and HPLC-MSn Approaches

“…Briefly, the fresh plant material (2 g) was placed in a 4 mL glass vial, which was sealed and left to equilibrate at room temperature for 1 h. Afterwards, the headspace was sampled with a Supelco SPME fiber coated with polydimethylsiloxane (PDMS, 100 µm) for 30 min. GC-MS analysis of the headspace extract was performed as described by Bendif et al [15], using a Varian CP-3800 gas chromatograph coupled to a Varian Saturn 2000 mass spectrometer. An Agilent DB-5 capillary column (30 m × 0.25 mm; coating thickness 0.25 µm) was used as the stationary phase.…”

“…Sample preparation was performed using a protocol previously described by Dall'Acqua et al [18] and Bendif et al [15]. A total of 20 g of the dried aerial parts were ground with an IKA A11 basic analytical mill to obtain a fine powder.…”

Phytochemical analysis of Clinopodium candidissimum (Munby) Kuntze growing in Algeria by an integrated HS-SPME-GC-MS, NMR and HPLC-DAD-MS n approach: valorisation of an endemic natural source of bioactive compounds

“…The extraction of C. candidissimum aerial parts was performed according to a previously published protocol (Dall'Acqua et al 2010;Bendif et al 2017). Briefly, 50 g of dried plant material were ground with a blender, suspended in 150 mL of methanol and extracted at r.t. for 15 min, by using an ultrasound bath.…”

“…Before analysis, the dried extract was dissolved in methanol at a concentration of 5 mg/mL, and the solution was filtered through a 0.45 µm Millipore filter. The HPLC-DAD-MS n method used was the same as reported in (Bendif et al 2017;Peron et al 2019).…”

“…Then, the SPME fibre was used to sample the headspace for 30 min. GC-MS analyses were achieved as described in (Bendif et al 2017)…”