Large-scale separation of clavine alkaloids from Ipomoea muricata by pH-zone-refining centrifugal partition chromatography.
Centrifugal partition chromatography in the pH-zone-refining mode was successfully applied to the separation of alkaloids, directly from a crude extract of Ipomoea muricata. The experiment was performed with a two-phase solvent system composed of methyl tert-butyl ether (MtBE)-acetonitrile-water (4:1:5, v/v) where triethylamine (10 mM) was added to the upper organic stationary phase as a retainer and trifluoroacetic acid (10 mM) to the aqueous mobile phase as an eluter. From 4 g of crude extract, 210 mg lysergol and 182 mg chanoclavine were obtained in 97% and 79.6% purities. Total yield recovery was >95%. Isolated alkaloids were characterized on the basis of their (1)H, (13)C NMR and ESI-MS data.
Maurya
Anupam
A
Analytical Chemistry Division, Central Institute of Medicinal and Aromatic Plants, Lucknow 226015, India.
Srivastava
Santosh Kumar
SK
D000097:Acetonitriles / Q000737:chemistry; D002853:Chromatography, Liquid / Q000379:methods*; D003377:Countercurrent Distribution; D004876:Ergot Alkaloids / Q000302:isolation & purification*; D006863:Hydrogen-Ion Concentration; D027741:Ipomoea / Q000737:chemistry*; D008738:Methyl Ethers / Q000737:chemistry
D000097:Acetonitriles; D004876:Ergot Alkaloids; D008738:Methyl Ethers; C043243:methyl tert-butyl ether; C032159:acetonitrile