Oasis max 1cc vac cartridge

For direct qualitative analysis, 100 mg of lyophilized plant material was extracted with 5 mL of MeOH: H₂O (8:2 v/v) in an ultrasonic bath for 20 min at 25 °C. The supernatant was collected and evaporated to dryness. Extracts were suspended in 2 mL of 0.2% formic acid (FA) in H₂O prior to preliminary purification and concentration using solid phase extraction (SPE). SPE was performed using an Oasis Max 1cc Vac Cartridge, 500 mg Sorbent per Cartridge, 30 µm Particle Size (Waters Corporation, Milford, MA, USA) conditioned with MeOH (4 mL) and H₂O (4 mL). The sample was loaded and cartridges washed with 5 mL water in 0.1% FA. The phenolic compounds were eluted with 5 mL of 80% MeOH in 0.1% FA. Samples were re-evaporated to dryness and dissolved in 25% of MeOH to obtain 1 mg dry weight/mL baseline plant material concentration.

4-iodobenzoic acid, N,N'-Dicyclohexylcarbodiimide (DCC), N-hydroxysuccinimide, tetrakis(triphenylphosphine)palladium (Pd(PPh₃)₄), tetrakis(pyridine)copper(II)triflate (Cu(OTf)₂Py₄), tetraethylammonium trifluoromethanesulfonate (N(Et)₄(OTf)), and solvents (dimethylacetamide, dichloromethane, ethyl acetate, methanol, heptane, toluene, and acetonitrile) were obtained from Merck KGaA (Sigma Aldrich brand, Darmstadt, Germany). Hexabutylditin was supplied from alfa aesar (Haverhill, MA, USA). N-succinimidyl 4-(tri-n-butylstannyl)-benzoate and 1-{[(4-Fluorophenyl)carbonyl]oxy} pyrrolidine-2,5-dione were purchased from abcr GmbH (Karlsruhe, Germany). Oasis WCX Plus Short Cartridge (225 mg Sorbent per Cartridge, 60 µm), Oasis HLB Plus Short Cartridge (225 mg Sorbent per Cartridge, 60 µm), Sep-Pak tC18 Plus Short Cartridge (400 mg Sorbent per Cartridge, 37–55 µm) and Oasis MAX 1 cc Vac Cartridge (10 mg Sorbent per Cartridge, 30 µm) were bought from Waters (Milford, MA, USA). PD-10 desalting column was acquired from Cytiva (Marlborough, MA, USA). Thin-layer chromatography (TLC) (normal phase plates, silica gel 60 coated with fluorescent indicator F254s) was obtained from Macherey–Nagel (Duren, Germany).