Journal: Journal of natural products
Article Title: Biochemometrics to Identify Synergists and Additives from Botanical Medicines: A Case Study with Hydrastis canadensis (Goldenseal)
Figure Lengend Snippet: LC-MS chromatograms (collected with ultraperformance liquid chromatography coupled to a Q-Exactive Orbitrap mass spectrometer) of a series of H. canadensis extract fractions. (A) Positive-ion electrospray mass spectrometry chromatogram of the crude extract after liquid–liquid partitioning. (B) The most active fraction (GS-4) of the crude extract shown in A after separation with flash chromatography over silica gel using a hexane–chloroform–methanol gradient (stage 1 separation). GS-4 was further fractionated using a second stage of flash chromatography over silica gel with a hexane–ethyl acetate–methanol gradient with GS-4-4 being the most active (C). GS-4-4-2 generated with stage 3 fractionation (using reversed-phase preparative HPLC with a water–acetonitrile gradient) (D). (E–H) The same H. canadensis extract and fractions analyzed using LC-MS in the negative-ion mode. Arrows represent the region of the chromatogram in which a given ion corresponding to a known constituent of H. canadensis (indicated by compound numbers) could be detected. Compounds 1 – 7 , 10 , 13 , 16 , 17 , 20 – 24 , and 28 while compounds 8 , 9 , 11 , 12 , 14 , 15 , 18 , 19 , and 25 – 27 29 is a new flavonoid that was isolated and identified based on NMR and MS data as part of this report. Red dotted arrows represent alkaloids and other compounds, while green dashed arrows represent flavonoids. In cases where a specific peak is not apparent in the chromatogram, the ion was identified based on mass spectrometric data.
Article Snippet: Extracts were suspended in 1:1 MeOH–dioxane (LC/MS grade, Fisher Scientific, Hampton, NH, USA) at either 1 or 0.1 mg/mL and subjected to ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) analysis via a Waters Acquity UPLC with an Acquity UPLC column (BEH C18 , 1.7 μ m, 2.1 × 50 mm, Waters Corporation, Milford, MA, USA) and a Thermo Q-Exactive Plus orbitrap mass spectrometer with heated electrospray ionization (Thermo Fisher Scientific, Milford, MA, USA).
Techniques: Liquid Chromatography with Mass Spectroscopy, Liquid Chromatography, Mass Spectrometry, Chromatography, Generated, Fractionation, High Performance Liquid Chromatography, Isolation, Nuclear Magnetic Resonance