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Fig. 4. SFC separation of Group IV (tangeretin group). (Peak 3, tangeretin; peak 4, 3,5,6,7,8,3’,4’-heptamethoxyflavone; SFC conditions, mobile phase 50% methano! (containing 0.25% diethylamine) and 50% liquid COz, flow rate, 70 mL/min; temperature, 30 °C; CO pressure, 100 bar; UV absorbance, 220 nm; column, DAICEL AD chiral column, 30mm x 250mm, 10 pm).

Figure 4 SFC separation of Group IV (tangeretin group). (Peak 3, tangeretin; peak 4, 3,5,6,7,8,3’,4’-heptamethoxyflavone; SFC conditions, mobile phase 50% methano! (containing 0.25% diethylamine) and 50% liquid COz, flow rate, 70 mL/min; temperature, 30 °C; CO pressure, 100 bar; UV absorbance, 220 nm; column, DAICEL AD chiral column, 30mm x 250mm, 10 pm).

Related Figures (5)

Fig. 1. Structures of four polymethoxyflavones isolated from sweet orange peel using SFC and chiral separation technology.
Fig. 1. Structures of four polymethoxyflavones isolated from sweet orange peel using SFC and chiral separation technology.
Fig. 2. Flow chart of PMF separation from OPE. The fractions at each group (Group I to Group VI in Fig. 2) were combined and concentrated. A small amount of residues of Groups IV (tangeretin group) and V (nobiletin group) was dissolved in acetonitrile, respectively. The dissolved solution was loaded onto a Cig reverse phase HPLC system. A gradi- ent method was used from 25% acetonitrile-75% water to 60% acetonitrile-40% water for 20 min with a flow rate of 20 mL/min. In an attempted separation of PMFs, several methods have been employed in preparative scale isolation of pure PMFs from orange peel extract. The most commonly used meth- ods including silica gel normal phase chromatography and Cig reverse phase HPLC encountered difficulty. Recently, by using high speed counter-current chromatography, five PMFs have been isolated from tangerine peel in milligram quanti- ties [20]. Chiral column based preparative HPLC has been reported to efficiently isolate gram scale quantity of nobiletin [21]. Although further investigation of large-scale separation of other PMFs using Chiral HPLC is still in process in our labo- ratory, the application of SFC technology in the separation of PMFs has been conducted. By using SFC technology, an effi- cient and scalable separation method was developed and a total
Fig. 2. Flow chart of PMF separation from OPE. The fractions at each group (Group I to Group VI in Fig. 2) were combined and concentrated. A small amount of residues of Groups IV (tangeretin group) and V (nobiletin group) was dissolved in acetonitrile, respectively. The dissolved solution was loaded onto a Cig reverse phase HPLC system. A gradi- ent method was used from 25% acetonitrile-75% water to 60% acetonitrile-40% water for 20 min with a flow rate of 20 mL/min. In an attempted separation of PMFs, several methods have been employed in preparative scale isolation of pure PMFs from orange peel extract. The most commonly used meth- ods including silica gel normal phase chromatography and Cig reverse phase HPLC encountered difficulty. Recently, by using high speed counter-current chromatography, five PMFs have been isolated from tangerine peel in milligram quanti- ties [20]. Chiral column based preparative HPLC has been reported to efficiently isolate gram scale quantity of nobiletin [21]. Although further investigation of large-scale separation of other PMFs using Chiral HPLC is still in process in our labo- ratory, the application of SFC technology in the separation of PMFs has been conducted. By using SFC technology, an effi- cient and scalable separation method was developed and a total
Fig. 3. SFC separation of Group V (nobiletin group). (Peak 1, nobiletin; peak 2, 5,6,7,4’-tetramethoxyflavone; SFC conditions, mobile phase 45% methanol (contain; 0.25% diethylamine) and 55% liquid COz, flow rate, 70 mL/min; temperature, 30°C; CO2 pressure, 100 bar; UV absorbance, 220 nm; column, DAICEL AD chira column, 30 x 250mm, 10 wm; a and c, start collection point; b and d, stop collection point).
Fig. 3. SFC separation of Group V (nobiletin group). (Peak 1, nobiletin; peak 2, 5,6,7,4’-tetramethoxyflavone; SFC conditions, mobile phase 45% methanol (contain; 0.25% diethylamine) and 55% liquid COz, flow rate, 70 mL/min; temperature, 30°C; CO2 pressure, 100 bar; UV absorbance, 220 nm; column, DAICEL AD chira column, 30 x 250mm, 10 wm; a and c, start collection point; b and d, stop collection point).
Fig. 5. Stack injection of SFC separation of Group V. (Total of 25 continuous injections, 80 mg of crude V per injection, other conditions in Fig. 4
Fig. 5. Stack injection of SFC separation of Group V. (Total of 25 continuous injections, 80 mg of crude V per injection, other conditions in Fig. 4
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ChemistryAnalytical ChemistryMedicineHigh Pressure Liquid ChromatographyLiquid Chromatography / Electrospray Ionization Mass SpectrometrySupercritical Fluid ExtractionSupercritical Fluid ChromatographySupercritical FluidBiochemistry and cell biologyPharmacology and pharmaceutical sciences
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