Skip to main content
. Author manuscript; available in PMC: 2010 Nov 1.
Published in final edited form as: Food Chem. 2009 Nov;117(2):375–380. doi: 10.1016/j.foodchem.2009.04.011

Table 1.

Composition of seven non-aqueous and five organic-aqueous solvent systems and summary of experimental results on separation of nootkatone in crude essential oil by HSCCC.

Solvent system (v/v)a KU/L (Valencene)b KU/L (Nootkatone)b α c Purityd (%)
 Sf (%)e
 Elution time (min)f
 tR (min)i
h – tg t – hh h – tg t – hh h – tg t – hh h – tg t – hh
Hex–CHCl3–ACN (6:2:5) 1.65 0.70 2.33 16.47 18.46 31.1 61.1 160–195 280–300 181 251
Hex–CHCl3–ACN (6:1:4) 4.46 0.63 7.22 53.93 64.98 82.3 83.0 105–135 305–350 139 298
Hex–CHCl3–ACN (10:1:10) 5.04 0.45 11.00 63.73 80.55 81.7 83.0 85–120 370–420 110 399
Hex–CH2Cl2–ACN (10:3:7) 1.97 0.65 3.00 53.87 64.82 75.2 70.0 230–270 275–315 147 274
Hex–CH2Cl2–ACN (10:1:10) 6.46 0.49 13.53 45.66 76.90 82.0 84.1 85–120 410–470 116 373
Hex–CH2Cl2–EtOAc–ACN (6:1:1:4) 2.48 0.72 3.45 29.02 70.45 45.2 66.4 150–180 255–300 175 250
Hex–CH2Cl2–EtOAc–ACN (10:1:1:10) 4.49 0.50 9.00 51.77 75.74 80.6 85.2 90–120 390–440 119 367
LtPet–(Et)2O–EtOH–H2O (5:0.5:4:0.5) 7.28 0.69 10.55 56.25 64.23 72.4 84.1 130–155 310–370 155 274
LtPet–EtOH–H2O (5:4:1) 28.64 0.95 30.17 75.87 61.85 79.2 86.9 160–185 180–230 192 209
LtPet–(Et)2O–EtOH–H2O (5:0.5:4:1) 31.50 1.14 27.63 66.36 55.44 76.7 87.6 300–380 180–240 221 177
Hex– EtOAc–MeOH–H2O (5:1:4:1) 28.68 1.11 25.84 75.51 55.26 82.2 91.2 185–210 145–170 218 182
Hex–MeOH–H2O (5:4:1) 93.56 1.25 74.85 77.39 29.55 81.3 92.6 190–220 140–200 241 163
a

Hex, n-hexane; ACN, acetonitrile; EtOAc, ethyl acetate; LtPet, light petroleum (30–60 °C); (Et)2O, diethyl ether; EtOH, ethanol; MeOH, methanol.

b

The partition coefficients (K): in head–tail elution using the lower phase as the mobile phase, the K value was expressed as KU/L = AU/AL, where AU and AL was the peak area of the compound in the upper phase and the lower phase by GC, respectively; whilst in tail–head elution using the upper phase as the mobile phase, the K value is the reciprocal of KU/L, that is 1/KU/L.

c

α is the separation factor obtained by the ratio of K values between valencene and nootkatone, e.g. α = KU/L (Valencene)/KU/L (Nootkatone).

d

Percentage of peak areas of nootkatone analysed by GC–MS.

e

Sf, retention of the stationary phase, Sf = Vs/VC, where Vs is the volume of the retained stationary phase, VC is the total column volume.

f

The time range of nootakone fraction being eluted out.

g

Head–tail elution mode, using the lower phase as the mobile phase.

h

Tail–head elution mode, using the upper phase as the mobile phase.

i

tR, the theoretical retention time of nootkatone, calculated by tR = VR/F and VR = VC[1 + (K – 1)Sf], where VR was the retention volume of nootkatone, F was the flow rate of the mobile phase and K was the partition coefficient of nootkatone.