| 分析方法 |
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| 儀器 |
Perkin Elmer series 200液相色譜儀 |
| 色譜柱 |
C8 色譜柱配置 5 μm 粒徑顆粒 (Spheri-5 RP-8, Brownlee, Perkin-Elmer), 25°C |
| 流動相 |
A: 乙腈: 水 = 80: 20, B: 1% 乙酸甲醇, 0-6 min 40% A 0.45 mL/min, 6-8 min 40-60% A 0.6 mL/min, 8-10.5 min 60-30% A 0.8mL/min, 10.5-15 min 30-20% A, 15-21 min 20-40% A. |
| 檢測器 |
UV λ244 nm 和 UV λ276 nm, API 3000 三重四極杆儀配備渦輪增壓離子噴霧接口, 負離子模式. |
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| 樣品製備 |
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方法一 |
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嶺南山竹子莖皮粉末由 95% EtOH 三次, 7 天, 乾燥置於水中備用, 石油醚 (3L)、氯仿 (9L)、BuOH (9L) 分餾。 |
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氯仿餾分上樣睢教主以石油醚: Me2CO = 7:1, 5:1, 3:1, 1:1, 0:1 洗脫得 3 餾分. 餾分 B 上樣矽膠柱石油醚: Me2CO = 5:1 至 2:1 洗脫.餾分 B2 進樣 Toyopearl HW-40C 柱, MeOH 洗脫. |
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RP-C18 色譜柱純化, MeOH: 水 = 65: 35 to 9 : 1 洗脫得目標化合物. |
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方法二 |
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乙酸乙脂 (5 L) 提取三次, 浸泡過夜並攪拌, 減壓蒸幹。 |
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矽膠色譜柱以庚烷-乙酸乙脂 = (95:5 - 50:50) 洗脫得 12 個餾分. 餾分 VI 上樣矽膠色譜柱庚烷-乙酸乙脂 = (90:10 - 75:25) 洗脫得黃色油狀物, 庚烷-乙酸乙脂 = (95:5 - 50:50) 再次色譜柱分離洗脫得10 個餾分. |
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餾分VII (350 mg) 上樣矽膠色譜柱庚烷-丙酮 (95: 5 to 50: 50)洗脫的 黃色油狀藤黃酚 (83 mg). |
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| 參考文獻 |
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|
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