化學名稱 補骨脂酚
外觀 淡黃色油狀液體
化學物質登錄號 10309-37-2
分子式
分子量 256.38
植物來源
生物活性
鑑定 旋光度 [α]30D +37.2°
1HNMR
分析方法
儀器 矽膠, HPTLC 板, 1 mm; Merck
流動相 20% (v/v) 乙酸乙酯/正己烷
檢測器 UV λ254 nm
儀器 Agilent1290 Infinity UPLC 儀 (Agilent Technologies, Santa Clara, CA)
色譜柱 Hypersil GOLD C4 色譜柱 (50 mm × 2.1 mm i.d., 粒徑1.9 µm, Thermo Fisher Scientific, Waltham, MA)
流動相 A: 0.1% 甲酸水, B: 0.1% 甲酸乙腈, 流率: 0.5 mL/min: 0 min, 30% B; 0.4-1.0 min, 90% B; 1.2 min, 30% B;0.3 min, 重新平衡時間
檢測器 正離子多反應監測ESI (MRM) 模式; 轉讓毛細管溫度: 320°C, 噴射電壓: 4000 V, 鞘氣: 25 psi, m/z 490 → m/z 171.1
儀器 Waters 515 Separations Module HPLC 儀及Waters 2487 二極管數組檢測器
色譜柱 Hypersil ODS2 色譜柱 (250 mm × 4.6 mm i.d., 5 µm; Dalian Elite Analytical Instrument Co. Ltd., Dalian, China)
流動相 甲醇: 水 (0.2% formic acid) = 90: 10, v/v;流率: 1.0 mL/min
檢測器 UV λ260 nm
儀器 泵 (Jasco, PU-2089, Tokyo, Japan) 和UV 檢測器 (Jasco, UV-2075)
色譜柱 XTerra™ RP18 色譜柱 (4.6 mm × 250 mm, 5 µm; Waters Co., MA, USA)
流動相 A: 0.1% 水-乙酸, B: 乙腈, 0-15 min 60% A, 15-35 min 60-50% A, 35-45 min 50-40% A, 45-55 min 40-30% A, 55-60 min 30-20% A, 1 mL/min
檢測器 UV λ245 nm
儀器 Agilent 1260 Infinity LC 儀及 DAD 檢測器
色譜柱 Alltima C18 色譜柱 (Alltech, 4.6 × 250 mm, 5 µm)
流動相 A: 乙酸水溶液, B: 乙腈, 0-15 min 40-50% B, 15-35 min 50-60% B, 35-55 min 60-80% B, 55-60 min 80% B, 1.0 mL/min
檢測器 UV λ251 nm
儀器 1100 HPLC 儀 (Agilent Technologies, California, USA)
色譜柱 DL-C18 色譜住 (5.0mm, 250 mm, 4.6 mm, Japan)
流動相 A: 乙腈, B: 0.01M 甲酸: 0-10 min 15-40% B, 10-30 min 40-55% B, 30-40 min 55-75% B, 40-60 min 75-80% B, 60-70 min 80-95% B, 15% A; 流率: 0.5 mL/min
檢測器 UV λ276 nm
樣品製備
方法一
補骨脂 (2.0 kg) 乾燥種子 95% EtOH 提取得 592 g 粗提取, 2.5 L 水中暫停 (392 g).
石油醚及乙酸乙酯分餾, 石油醚部中餾分PE (143 g) 和乙酸乙酯中餾分 EA (120 g).
餾分 EA (100 g) 上樣矽膠色譜柱 (CC) 以石油醚及提督增加的丙酮洗脫得餾分 1-9, TLC 顯色. 餾分1-4 (共 46 g) 主要含有補骨脂酚。
參考文獻
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連結 中藥材圖像數據庫 藥用植物圖像數據庫 中藥標本數據庫

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