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13 COUNTER-CURRENT CHROMATOGRAPHY Sample Solvents Solvent system Ratio Mobile phase Silymarin n-Hexane–EtOAc–MeOH–H 2O 1:4:3:4 Lower Lignans Arctiin EtOAc–1-BuOH–EtOH–H 2O 10:1:2:10 Lower Lignan diglucoside MTBE–1-BuOH–CH 3CN–H 2O 1:3:1:5 Upper Coumarins Psoralen and isopsoralen n-Hexane–EtOAc–MeOH–H 2O 10:7:10:8 Lower Infl acoumarin A n-Hexane–CHCl 3–MeOH–H 2O 5:6:3:2 Lower Chalcones Licochalcone A n-Hexane–CHCl 3–MeOH–H 2O 3:12:6:4 Lower Quinones Tanshinones n-Hexane–EtOH–H 2O (a) 20:11:9 Lower (b) 10:7:3 Shikonin n-Hexane–EtOAc–EtOH–H 2O 16:14:14:5 Lower Diterpene quinone n-Hexane–CCl 4–MeOH–H 2O 1:3:3:2 Lower Monoterpenes Monoterpenes and monoterpene glycosides CHCl 3–MeOH–H 2O 7:13:8 Upper Iridoid glycosides CHCl 3–MeOH–1-PrOH–H 2O 5:6:1:4 Lower Sesquiterpenes Artemisinine, artemisitene arteannuin B n-Hexane–EtOAc–EtOH–H 2O 6:4:5:4 Lower Diterpenes 10-Deacetylbaccatin III n-Hexane–EtOAc–EtOH–H 2O 2:5:2:5 Lower n-hexane–CHCl 3–MeOH–H 2O 5:25:34:20 Lower Trachylobanes and isopimaranes n-Heptane–CH 3CN–CH 2Cl 2 10:7:3 Lower Triterpenes Celastrol n-Hexane–EtOAc–CCl 4–MeOH–H 2O1:1:8:6:1 Lower Saponins Ginsenosides CHCl 3–MeOH–2-BuOH–H 2O 5:6:1:4 Lower EtOAc–1-BuOH–H 2O 1:1:2 Upper 222
EXTRACTION TECHNOLOGIES FOR MEDICINAL AND AROMATIC PLANTS Sample Solvents Solvent system Ratio Mobile phase n-Hexane–1-BuOH–H 2O 3:4:7 Lower Phytolacca saponins CHCl 3–MeOH–2-PrOH–H 2O 5:6:1:4 Lower Glycyrrhizin EtOAc–MeOH–H 2O 5:2:5 Lower Carotenoids Zeaxanthin n-Hexane–EtOAc–EtOH–H 2O 8:2:7:3 Lower Lycopene n-Hexane–CH 3CN–CH 2Cl 2 20:13:7 Upper Alkaloids Aporphine alkaloids CH 2Cl 2–MeOH–5% HOAc 5:5:3 Lower Naphthylisoquinoline alkaloids CHCl 3–EtOAc–MeOH–0.1 M HCl 5:3:5:3 Lower Diterpene alkaloids n-Hexane–CH 2Cl 2–MeOH–H 2O 15:15:24:8 Lower C 6H 6–CHCl 3–MeOH–H 2O 5:5:7:2 Lower Tetramethylpyrazines Chuanxiongzine n-Hexane–EtOAc–EtOH–H 2O 5:5:3:7 Lower Glucosinolates PrOH–CH 3CN–(NH 4) 2SO 4–H 2O 10:5:12:10 Upper Cyclodepsipeptides n-Heptane–EtOAc–MeOH–H 2O 2:8:2:8 Lower 13.5.1.2 Retention of the Stationary Phase • Successful separation in HSCCC-CPC largely depends on the amount of the stationary phase retained in the column. In general, higher the retention of stationary phase, better the peak resolution. • The amount of stationary phase retained in the column is highly correlated with the settling time of the two phases in a test tube. • Measure the settling time of the two-phase solvent system to be used for the separation. • The procedure is as follows: the two phases are fi rst equilibrated in a separatory funnel. Deliver 2 ml of each phase, a total volume of 4 ml, into a test tube or graduated cylinder, which is then capped. Gently invert the container for several times and then immediately place it in an upright position to measure the time required for the two phases to form clear layers with a distinct interface. • If the settling time is less than 20 seconds, the solvent system will provide satisfactory retention of the stationary phase, usually over 50% of the total column capacity, in a proper range of flow rates. 223
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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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