Tlc plates silica gel 60 f254

Dried and cut leaflets (Lot 26094) and pods (Lot 22421) were obtained from Alfred Galke GmbH (Bad Grund, Germany). Retard tablets (Sennalax^®, Lot 2014211) were bought in a local pharmacy. SPE cartridges (Chromabond HR-XA, 85 µm, 3 mL/500 mg) and a 70 mL reservoir column were obtained from Macherey-Nagel GmbH (Düren, Germany), and cartridges for flash chromatography (Flashpure Ecoflex Silica SL 50 μm irregular 10 g, Lot 150317B) were ordered from Büchi (Flawil, Switzerland). Dimethyl sulfoxide-d₆ (99.80%, lot S1051, batch 0119E) for NMR spectroscopy was purchased from Eurisotop GmbH, Saarbrücken, Germany, and conventional 5 mm sample tubes were obtained from Rototec-Spintec GmbH, Griesheim, Germany. LCMS-grade acetonitrile, gradient-grade methanol, analytical-grade solvents, and TLC plates (silica gel 60 F254) were purchased from VWR International GmbH, Darmstadt, Germany. Hydrochloric acid (34%) and trifluoroacetic acid (TFA) were obtained from Carl Roth GmbH (Karlsruhe, Germany), acetic acid was purchased from Thermo Fisher Scientific Inc. (Waltham, MA, USA), and LCMS-grade formic acid was purchased from Merck (Darmstadt, Germany). Water was doubly distilled in-house.

LC-MS grade formic acid, Diaion HP-20, and Sephadex LH-20 were purchased from Sigma Aldrich Co., St. Louis, MO, USA. Silica gel (40–63 μm) for column chromatography, TLC plates (silica gel 60 F254), acetonitrile and water (both of LC-MS grade), gradient grade methanol, and other (analytical grade) solvents were obtained from VWR International GmbH, Darmstadt, Germany. Water used for isolation was doubly distilled in-house. Apigenin (14, Lot A002/02-08) and luteolin (15, Lot L007/02-08) were obtained from TransMIT, Marburg, Germany. Solid phase extraction (SPE) columns (Chromabond HR-XA 3 mL/500 mg) were obtained from Macherey-Nagel GmbH and Co. KG, Düren, Germany. Dimethyl sulfoxide-d₆ (99.80%, Lot S1051, Batch 0119E) and methanol-d₄ (99.80%, Lot P3021, Batch 1016B) for NMR spectroscopy were purchased from Euriso-top GmbH, Saarbrücken, Germany, and conventional 5 mm NMR sample tubes were obtained from Rototec-Spintec GmbH, Griesheim, Germany.