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自制奶酪

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The powdered seeds of A. tuberosum (50 kg) were extracted successively with petroleum either×2 and 95% EtOH×3. After evaporation of ethanol in vacuo, the residue was suspended in water and then extracted successively with petroleum ether, EtOAc and n-BuOH. The n-BuOH fr. (270 g) was subjected to Diaion HP-20 using an EtOH–H2O gradient system (0–100%). The fr. (60 g) eluted by 70+30% EtOH was subjected to silica gel CC with a CH2Cl2–MeOH–H2O solvent system (5:1:0.15–1:1:0.3). The fr. eluted by CH2Cl2–MeOH–H2O (4:1:0.2) was subjected to RP-18 silica gel CC with 70 and 75% MeOH to get compounds 1 (170 mg) and 2 (250 mg); the fr. eluted by CH2Cl2–MeOH–H2O (3:1:0.2) was subjected to RP-18 silica gel CC with 70% MeOH to afford compound 3 (250 mg).

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自制奶酪: 金币+15, 翻译EPI+1, ★★★很有帮助 2015-12-14 15:54:18
The powdered seeds of A. tuberosum (50 kg) were extracted successively with petroleum either×2 and 95% EtOH×3. After evaporation of ethanol in vacuo, the residue was suspended in water and then extracted successively with petroleum ether, EtOAc and n-BuOH. The n-BuOH fr. (270 g) was subjected to Diaion HP-20 using an EtOH–H2O gradient system (0–100%). The fr. (60 g) eluted by 70+30% EtOH was subjected to silica gel CC with a CH2Cl2–MeOH–H2O solvent system (5:1:0.15–1:1:0.3). The fr. eluted by CH2Cl2–MeOH–H2O (4:1:0.2) was subjected to RP-18 silica gel CC with 70 and 75% MeOH to get compounds 1 (170 mg) and 2 (250 mg); the fr. eluted by CH2Cl2–MeOH–H2O (3:1:0.2) was subjected to RP-18 silica gel CC with 70% MeOH to afford compound 3 (250 mg).
50公斤粉碎后的韭菜籽先后用石油醚抽提两次,95%乙醇抽提三次。乙醇抽提液蒸干后,残留物先后用水悬浮,再先后用石油醚,乙醇和正丁醇萃取。正丁醇萃取组分(270g)上Diaion HP-20柱,用EtOH–H2O(0-100%)浓度递度分离。70%乙醇-30%水洗脱组分再用硅胶层析, CH2Cl2–MeOH–H2O溶剂系统 (5:1:0.15–1:1:0.3)分离。从CH2Cl2–MeOH–H2O (4:1:0.2) 得到的组分用逆相RP-18硅胶层析分离,用70%和75%乙醇洗脱,得到化合物1 (170mg)和2(250mg); 从CH2Cl2–MeOH–H2O (3:1:0.2)得到的组分用逆相RP-18硅胶层析分离, 用70%乙醇洗脱,得到化合物3 (250mg) 。
离成功还差一点
2楼2015-12-14 15:08:48
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