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13 COUNTER-CURRENT CHROMATOGRAPHY When the polarity of the target compounds is unknown, the search may start with the two-phase solvent system composed of hexane– ethyl acetate–methanol–water at a volume ratio of 3:5:3:5, which has a moderate degree of polarity. If the partition coeffi cient is slightly off from the proper range, it can be adjusted by modifying the volume ratio. For example, if K U/L is slightly over 2, the volume ratio may be modifi ed toward more hydrophobic such as 3.2:5:3.2:5, and if K U/L is slightly less than 0.5, the volume ratio may be modifi ed in the opposite direction to 2.8:5:2.8:5. If the target compound is mostly distributed in the upper organic phase, the search is directed upward along the arrow. If it is mostly distributed in the lower aqueous phase, the search is directed downward along the arrow. If the sample is an extract of plant material, the search may start at any point according to the polarity of the solvent used for the extraction. If the sample is an ethyl acetate extract (relatively hydrophobic solvent), the search may start at hexane–ethyl acetate–methanol–water (1:1:1:1), whereas if the sample is a methanol extract (polar solvent), the search may start at 1-butanol–water. The search should be continued until a suitable range of K U/L values for all of the compounds of interest is obtained. 13.5.1.1 Solvent Systems for the Separation of a Large Variety of Natural Products Table 2 presents different kinds of solvent systems that have been used for the separation of a large variety of natural products, which may be of immense importance for the researcher to fi nd a suitable solvent system for the desired separation of natural products. Table 2: Solvent systems used for the separation of natural products Sample Solvents Solvent system Ratio Mobile phase Aryl ketones Phenylethanone derivatives n-Heptane–EtOAc–MeOH–H 2O 4:2:2:1 Lower Styrylpyrones Kava lactones n-Hexane–acetone–MeOH–H 2O 4:1:3:1 Upper Benzofurans Dibenzofurans n-Heptane–CH 2Cl 2–CH 3CN 10:3:7 Lower, upper 220
EXTRACTION TECHNOLOGIES FOR MEDICINAL AND AROMATIC PLANTS Sample Solvents Solvent system Ratio Mobile phase Phenolic glycosides Gastrodin EtOAc–1-BuOH–H 2O 3:2:5 Lower Phenylpropanoids Honokiol, magnolol n-Hexane–EtOAc–MeOH–H 2O 5:2:5:2 Lower Phenylpropanoid glycosides Verbascoside EtOAc–CH 3CN–H 2O 13:13:24 Lower Acteoside EtOAc–H 2O 1:1 Lower Hydrolyzable tannins Ellagic acid and corilagin 1-BuOH–HOAc–H 2O 4:1:5 Lower Catechins Epigallocatechin n-Hexane–EtOAc–H 2O 1:9:10 Lower Tea catechins n-Hexane–EtOAc–MeOH–H 2O 3:10:3:10 Lower Proanthocyanidins Tea proanthocyanidins n-Hexane–EtOAc–MeOH–H 2O 1:5:1:5 Lower Anthocyanins MTBE–1-BuOH–CH 3CN–H 2O 2:2:1:5 Lower Bilberry anthocyanins MTBE–1-BuOH–CH 3CN–H 2O–TFA 1:4:1:5:0.01 Lower Flavonoids Flavones and chalcones CHCl 3–CH 2Cl 2–MeOH–H 2O 2:2:3:2 Lower CH 2Cl 2–MeOH–CH 3CN–H 2O 40:11:25:20 Lower EtOAc–1-PrOH–H 2O 140:8:80 Upper Flavonoid glycosides n-Hexane–EtOAc–MeOH–H 2O 1:8:1:8 Lower n-Hexane–EtOAc–MeOH–H 2O 2:12:3:15 Lower CHCl 3–MeOH–H 2O 8:7:4 Lower C-Glycosyl fl avones CHCl 3–MeOH–H 2O 6:25:29 Lower EtOAc–1-BuOH–MeOH–H 2O 35:10:11:44 Lower Icariin n-Hexane–1-BuOH–MeOH–H 2O 1:4:2:6 Lower Isofl avone glycosides EtOAc–1-BuOH–EtOH–H 2O 30:10:6:50 Lower EtOAc–EtOH–HOAc–H 2O 16:4:1:20 Lower Flavonol glycosides 1-BuOH–H 2O 1:1 Lower Flavonolignans 221
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Extraction Technologies for Medicin
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CONTRIBUTORS Chapter 6 Aqueous Alco
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EXTRACTION TECHNOLOGIES FOR MEDICIN
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7 DISTILLATION TECHNOLOGY FOR ESSEN
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9 SOLID PHASE MICRO-EXTRACTION AND
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