2002-2003 > Academic research: refereed > Publication in refereed journalVersion of RecordPublishe

Qian, ZM

Yuan, QP

Zhang, H

PolyU Institutional Repository

? 21?　? 3?2002?　　8? ?　?　?　?SOYBEAN　SCIENCEVol.21　No.3Aug.　　2002　　　??? CO2?????????????? ???1　?　?1　???2(1.???????????? ,?? 100029;2.????????????????? ,??)??　测定了大豆异黄酮中两种主要成分染料木甙和大豆黄甙的雾点压力 ,采用有机溶剂提取和超临界 CO2 抗溶剂技术通过两次膨胀进行大豆异黄酮的精制 ,得到的产品中大豆异黄酮含量高于90%,异黄酮收率大于 78%。该研究为超临界 CO2 抗溶剂技术在天然极性物质分离纯化中的应用提供了新的思路 。???　超临界流体;抗溶剂;大豆异黄酮?????　S565.1　　?????　A　　????　1000-9841(2002)03-0177-060　??????? (soybean isoflavone)????????? ,???α-???????????? ,???????? ,?? 12??? ,????????????(genistin)?????(daidzin)?????? 80%?? ,????[ 1] :R1=O-gluco syl , R2=H , R3=OH ?????R1=O-glucosyl , R2=H , R3=H ???????????? ,???????????????? ,?????? 、???? ,??????? ,??????? ,?????????? ,????????????[ 2 , 3]??ADM ??? 1996?????? 20? 40%????????? ,??????????? ,???????? 。???????????????????????????? ,???? ,??????。??????????????????? 、???????????[ 4-7] ,?????????? 、????????? ,????????????? 。???? 、????????????????????????。??????????????????????????????? ,????????? ,????????? ,???????????????????????????。???????????????????? ,???????????????????? ,????????? ,??????? 。?? ,????????????????????????? ,???????????????? 。Gallagher?[ 8]? 1989???????????????? ,?? ,??????????????? ,?????? 、??????????????????????。????????? ,???????? ,??????? CO2??。?????? ,??????????????????????。????????-?????????? ,??????????????????????????????。1　?????1.1　??????? ????:2001-12-28　????:???(1969-),? ,?? ,????????。1.1.1　???????? 1???????? ,??????????????? ,??? 50mL ,????????。??????????-?????????? ,????????CO2 , ??????????1-???　2-???　3-????　4-?????? 1　????????Fig.1　Meansured of balance? ,?????????????????????。???????????? CO2 ????????? 。1.1.2　??? CO2 ??????????2? CO2 ???????????? ,???????????? 100mL ??????????? ,????????????? ,????100???? ,???????????? 。??????????-??????????? ,?240mL/h????? CO2 ,??????????? ,???????????????? ,????????????? ,?????????????????? , ???? , ???? , ??20min ,???????????????。?????? ,????????? , ??????CO2 ,???????????。?????? ,????? ,????????????????。???????????????????? ,????????。1-CO2 ??　2-?????　3-????　4-????　5-?????　6-?????? 2　CO2 ????????????Fig.2　Expariment of CO2 antisolvent process1.1.3　?????????※???? ※??? CO2 ?????　　　　　　　　 　　　　　　　 　　　　　　　　　　　　　　↑　　　　　　　　　　　　↑　　　　　　???? 　　　　　　　　　????　　　　　　 　　↑　　　　　　??? CO2????? ※???? ※??1.2　????????????? 10.57%(??????? 4.81%,????? 3.70%,?????????? 2.06%),?????? 107???? 。CO2 ??? 99.9%,?????????? 。1.3　?????????? HPLC ????(?????????)。????:?? ,45℃;??? , 30%??+70%?????(???? 5%),?? , 1ml/min;??178 　　　　　　　　　　　　　　　?　?　?　?　　　　　　　　　　　　　　　　　　　　　　　　3?? ,SPD-6AV ,???? 254nm 。??:C18??? ,? 250 mm , ?? 4.6mm 。????(genistin)?????(daidzin)??????? Sigma???? 。2　?????2.1　????????????????????????????????????????????????????????????? ,??????????? 。?? ,??? 1 ???????????? 308.15K ?318.15K????????????????????????????。????-???????????? 3?? 。? 3　?????????????Fig.3　The data of phase equilibium of genistin in aceton　　??????? ,?????? ,??????。?????????? ,???????????????????????? ,????????????????????。?? 3??????????????? 0???????? ,????? ,?? 308.15K ? 318.15K??????? 4.91? 4.83MPa。? 4　?????????????Fig.4　The data of phase equilibrium of daidzin in aceton1793?　　　　　　　　　　　　　　　　　????:???CO 2 ??????????????　　???????????????? 308.15K?318.15K ????????? 4.89 ? 4.81M pa(? 4)。????????? ,?????????????。?????????????????????D????? G ???????????。??????????????-???? ,??????????????????????? ,???????????? ,?????????????????????????? ,????????????????? ,???????? ,?????????。2.2　????????????????2.2.1　????????-?????? ,?????????????? 。??????? ,????????????? ,???? CO2 ??????????? 。????? 85%? 95%???????????????? ,HPLC ???? ,??? 85%??????????????????????。??????????? 1.3mg/mL ,????????? 1 mg/mL。2.2.2　CO2 ???????10%?????????????? ,??? 、?? 、? 、?? 、????????。?????????? ,????????????????????? ,?? 4??。Ⅰ Ⅱ Ⅲ——— ——— ——— ——— ——— ——— ——— ——— ——— ——— ——— ——— ———※????? 5　??????????????Fig.5　Sample of soybean isoflavone?? Ⅱ????? , Ⅰ? Ⅲ????????????????????? 。????????????????????? ,???? CO2 ??? ,????????????? ,???????????Ⅰ?????? ,??? CO2 ??????????????? ,???????(????????),??????????。?????????????????? , ??? 308.15K ?318.15K?????????????? ,????1??。?????????????????:???(%)=(????/????)×100%????=(V-V0)/V0?? V0 ? V???????????? 。???????:?????????????? ,?????????? ,?????????:????????=(1-???)×?????????????/????????×100%???????????????? ,?????????? ,???????:????????=???×?????????????/????????×100%??????=????????×?????????????????????????:????????=???×?????????????+(1-???)×???????????? 。?? 1???? ,???????????????????????????? ,?????? ,???? CO2???????????????? 。????????????????????? 2.48 ,?? CO2 ??? 3.73MPa ,????????????????????? 。???????????? Ⅰ ,???????? ,????????????????????????? ,??Ⅰ?????? ,?????????? ,??CO2???????? ,????????????? ,?????????????? 。?? ,?? 308.15K? 318.15K ?????????? ,??????????? ,308.15K ??????????? ,????? 308.15K ?? ,???? ,????? ,??????????? 。?? 1????? ,? CO2 ???????????? ,?????? 10%??? 40%(308.15K ,???? 2.48 , 85%??),???????89.6%,????????????(?????????)????????? ,????????67%(?? 107????)? 58%(?????????? 、??????????)。??? 1 ??? , CO2 ???????????????????? I ????????????? ,??????? ,??????????????? ,?????????????? ,????180 　　　　　　　　　　　　　　　?　?　?　?　　　　　　　　　　　　　　　　　　　　　　　　3???? Ⅲ???。?? ,????????????? 2.5?? ,?????? 308.15K ,????85%??。?????????????? ,????????????????????????。? 2????????????????。? 1　CO2 ??????????????????????(85%??)Table 1　CO2 antisolv ent process for primary purification soy isoflavone??????????? ???????G(%) D(%) ????(%)???(%) G(%) D(%)????(%)308.15 K318.15 K1.30 8.33 6.29 18.03 43.39 0.22 0.32 0.711.72 10.18 7.62 21.96 54.36 0.29 0.41 0.892.08 11.59 8.53 24.72 60.24 0.33 0.52 1.132.48 19.62 14.19 40.89 76.97 0.38 0.56 1.423.52 15.94 7.62 26.44 84.06 2.76 2.96 8.123.95 4.41 3.19 8.33 86.49 4.87 3.78 10.921.48 7.91 6.01 17.21 40.55 0.26 0.31 0.681.69 9.34 7.20 20.63 51.21 0.30 0.36 0.872.19 12.20 9.11 25.91 62.38 0.36 0.42 1.222.34 16.53 12.84 35.36 73.33 0.39 0.45 1.473.06 9.64 6.17 23.68 80.31 3.67 3.12 7.283.87 8.42 6.01 15.90 82.80 4.05 3.22 9.39? 2　CO2 ??????????????????????(85%??)Table 2　CO2 antiso lvent process for second purification soy isoflavone??????????? ??????????(%)G(%) D(%) ????(%) G(%) D(%)????(%)308.15 K2.58 1.97 32.16 50.34 98.53 19.37 13.43 39.733.01 14.7 36.72 37.69 96.78 16.45 10.11 31.343.46 33.06 48.69 37.88 94.54 7.26 3.96 14.624.01 39.59 43.52 32.02 90.23 3.96 2.46 8.56　　?? 2 ???? ,????????? 4.01? ,?????????????? 90%,?????????????? 10%?? ,????????????。???? 40%??? 90%,???87.3%。10%???????????? CO2????? ,????? 90.23%,???? 78.2%。?????????????? 90%??????????????。3　??CO2 ???????????????? ,???????? 10%??? 90%?? ,????74%?? ,????????????????? ,??????? ,???????? ,???????????? ,?????????????????????????? 。CO2 ?????? CO2 ????????????????? ,????????????????? ,??????????????。??????????????????? ,????????。?????????? ,?????????? 、?????????????????? 。?　?　?　?1　Naokazu Ohta , Goro Kuwata , et al.Isoflavonoid Constituents ofSoybeans and Isolation of a New Acetyl Daidzin[ J] .Agic.Biol.Chem.1979 , 43(7):1415-1419.1813?　　　　　　　　　　　　　　　　　????:???CO 2 ??????????????2　Kelly , Graham , Edmund.Health S upplements Containing Phy to-oe-strogens[ P ] .Analogues or Metabolites Thereof , WO 93/ 23069 ,Nov.25 , 1993.3　Greg Peterson , S tephen Barnes.Genistein Inhibiti on of the Grow thof Human Breast Cancer Cells:Independence f rom Est rogen Recep-tors and the Multi-drug Resistance Gene[ J] .Biochemical and Bio-physical Research Communicat ions , 1991 , 179(1):661-667.4　Naokazu Ohta , Goro Kuwata , et al.Isoflavonoid Constituents ofSoybeans and Isolation of a New Acetyl Daidzin[ J] .Agic.Biol.Chem.1979 , 43(7):1415-1419.5　Yukio Ohshima , Toru Okuyama , et al.Isolation and High Perfor-m ance Liquid Chromatography (HPLC)of Isoflavonoids from thePueraria Root[ J] .Planta medica.1988:250-254.6　BoLin Zheng.Superior:John A.Yegge , Longmon , et al.Processfor the Isolat ion and Purification of Isof lavones[ P] .US 5 , 679 , 806 ,Oct.21 , 1997.7　Eric T.Gugger , Daniel G.Dueppen.Production of Isoflavone En-riched Fract ions f rom Soy Protein Ext racts [ P ] .US5 , 702 , 752 ,Dec.30 , 1997.8　Gallagher P.M., Coffey M.P., Krukonis V.J., et al.Gas anti-solvent recrystallizat ion:new process to recrystallize compounds in-soluble in supercritical f luids[ P] .ACS Symp.Series , 406, 1989 ,334.STUDY ON THE PURIFICATION OF SOY ISOFLAVONE BYSUPERCRITICAL CO2 ANTISOLVENT PROCESSYuan Qipeng 1　Zhang Huai1　Qian Zhongming2(1.College of Chem ical Engineering , Beij ing University of Chemical Technology , Beij ing 100029;2.Department of Applied Biology &Chem ical Technology , The Hong Kong Polytechnic University)Abstract　The data of phase equilibrium of genistin and daidzin in aceton was measured.The super critical CO2anti-solvent process and ex traction by o rganic solvent was combined to purify soy isof lavone.The content ofisoflavone in the product is higher than 90% and the y ield is 78%.This study provides a new idea for purifyingnatural product by means of super critical CO2 anti-solvent process.Key words　Super critical fluid;Anti-solvent;Soy isoflavone　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　　2003?《????》????《????》? 1992??????????????????????????。《????》????????? ,??????????? 。????:???? 、????? 、???? 、???? 、???? 、???? 、???? 、???? 、???? 、????????????? 、??????????。???? 、?????????????。??????? 。?? ,???? 25???。?????(210mm×297mm)。???? CN22-1201/S ,????:?? 7.00? ,?? 28.00?。????:12-137。??????(?)????。?????????????????? 6? ,????????《????》????? ,?? 136100 。《????》???? 、?? 、???????????????? 。? 2001????????? 。???????:??? 050104?。??:0434-6257334 ,E-mail:ymkx@cjaas.com182 　　　　　　　　　　　　　　　?　?　?　?　　　　　　　　　　　　　　　　　　　　　　　　3?

Study on the purification of soy isoflavone by supercritical CO2 antisolvent process

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