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Extraction Technologies for Medicinal and Aromatic ... - Capacity4Dev

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EXTRACTION TECHNOLOGIES FOR MEDICINAL AND AROMATIC PLANTS<br />

Sample<br />

Solvents<br />

Solvent system<br />

Ratio<br />

Mobile<br />

phase<br />

n-Hexane–1-BuOH–H 2O 3:4:7 Lower<br />

Phytolacca saponins CHCl 3–MeOH–2-PrOH–H 2O 5:6:1:4 Lower<br />

Glycyrrhizin EtOAc–MeOH–H 2O 5:2:5 Lower<br />

Carotenoids<br />

Zeaxanthin n-Hexane–EtOAc–EtOH–H 2O 8:2:7:3 Lower<br />

Lycopene n-Hexane–CH 3CN–CH 2Cl 2 20:13:7 Upper<br />

Alkaloids<br />

Aporphine alkaloids CH 2Cl 2–MeOH–5% HOAc 5:5:3 Lower<br />

Naphthylisoquinoline<br />

alkaloids<br />

CHCl 3–EtOAc–MeOH–0.1 M HCl 5:3:5:3 Lower<br />

Diterpene alkaloids n-Hexane–CH 2Cl 2–MeOH–H 2O 15:15:24:8 Lower<br />

C 6H 6–CHCl 3–MeOH–H 2O 5:5:7:2 Lower<br />

Tetramethylpyrazines<br />

Chuanxiongzine n-Hexane–EtOAc–EtOH–H 2O 5:5:3:7 Lower<br />

Glucosinolates PrOH–CH 3CN–(NH 4) 2SO 4–H 2O 10:5:12:10 Upper<br />

Cyclodepsipeptides n-Heptane–EtOAc–MeOH–H 2O 2:8:2:8 Lower<br />

13.5.1.2 Retention of the Stationary Phase<br />

• Successful separation in HSCCC-CPC largely depends on<br />

the amount of the stationary phase retained in the column.<br />

In general, higher the retention of stationary phase, better<br />

the peak resolution.<br />

• The amount of stationary phase retained in the column is highly<br />

correlated with the settling time of the two phases in a test tube.<br />

• Measure the settling time of the two-phase solvent system<br />

to be used <strong>for</strong> the separation.<br />

• The procedure is as follows: the two phases are fi rst equilibrated<br />

in a separatory funnel. Deliver 2 ml of each phase, a<br />

total volume of 4 ml, into a test tube or graduated cylinder,<br />

which is then capped. Gently invert the container <strong>for</strong> several<br />

times <strong>and</strong> then immediately place it in an upright position to<br />

measure the time required <strong>for</strong> the two phases to <strong>for</strong>m clear<br />

layers with a distinct interface.<br />

• If the settling time is less than 20 seconds, the solvent system will<br />

provide satisfactory retention of the stationary phase, usually over<br />

50% of the total column capacity, in a proper range of flow rates.<br />

223

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