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植物來源 |
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生物活性 |
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鑑定 |
旋光度 |
[α]18D-60.5 (c, 0.5 氯仿)
[α]24D-43.2 (乙醇) |
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| 分析方法 |
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| 儀器 |
矽膠60 F254製備TLC 板 (1.0 mm, 20 x 20 cm, E. Merck, Darmstadt, Germany) |
| 流動相 |
石油醚: 乙酸乙酯 = 85 : 15, v/v |
| 檢測器 |
UV λ280 nm |
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| 儀器 |
Agilent 1290 UPLC 系統 (Agilent Technologies, Waldbronn, Germany), 和Aglient 6520 Q-TOF質譜 (Agilent Corporation, Santa Clara, CA, USA) ESI源連接Agilent 1290 UPLC, Waters Acquity UPLC™ 儀器 (Waters Corporation, Milford, MA, USA) 及DAD檢測器定性分析 |
| 色譜柱 |
ZORBAX SB-C18 色譜柱 (100 mm × 4.6 mm, 1.8 μm, Agilent), 50°C |
| 流動相 |
A: 0.1% 甲酸水, B: 乙腈, 0-7 min 5-17% B, 7-14 min 17-25% B, 14-16 min 25-28% B, 16-22 min 28-30% B, 22-33 min 30-85% B, 33-40 min 85-95% B, 0.4 mL/min. |
| 檢測器 |
正負離子模式, 乾燥氣 (N2): 10.0 L/min 350°C, 霧化氣: 40 psig, 毛細管: 4500 V, 碎片: 150 V, 撇渣氣: 65 V, 八極RF: 750 V |
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| 儀器 |
Agilent 1290 UPLC 系統 (Agilent Technologies, Waldbronn, Germany), 和Aglient 6520 Q-TOF 質譜 (Agilent Corporation, Santa Clara, CA, USA) ESI 連接 Agilent 1290 UPLC儀. Waters Acquity UPLC™ 儀器 (Waters Corporation, Milford, MA, USA) 及 DAD 檢測器定性分析. |
| 色譜柱 |
ZORBAX SB-C18 色譜柱 (100 mm × 4.6 mm, 1.8 μm, Agilent), 50°C |
| 流動相 |
A: 0.1% 甲酸水, B: 乙腈, 0-7 min 5-17% B, 7-14 min 17-25% B, 14-16 min 25-28% B, 16-22 min 28-30% B, 22-33 min 30-85% B, 33-40 min 85-95% B, 0.4 mL/min. |
| 檢測器 |
UV λ230 nm, UV λ250 nm, UV λ280 nm |
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| 儀器 |
Shimadzu LC-20AVP 系統配備兩個 LC-20AT 容積系統, SPD-M20AVP UV-vis 光電二極管數組檢測器, Model 7725 進樣閥和 20 μL 回路, 自動進樣器, SCL-20AVP 控制系統, Class-VP-LC 工作站 (Shimadzu, Kyoto, Japan). |
| 色譜柱 |
Apollo C18 色譜柱 (150 × 4.6 mm I.D., 5 μm), 30°C |
| 流動相 |
A: 甲醇, B: 0.05% H3PO4, 0-3 min 45-40% B, 3-17 min 40-33% m, 17-43 min 33%, 1 mL min |
| 檢測器 |
UV λ254 nm |
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| 儀器 |
Agilent 1100 series HPLC-DAD 系統包括真空脫氣機, 二元泵, 自動進樣器, 恒溫柱溫箱, DAD 檢測器 (Hewlett Packard, U.S.A.) 及 UV 色譜採集. |
| 色譜柱 |
Alltima C18 色譜柱 (5μm, 4.6mm × 150 mm, Alltech Associates, Inc., U.S.A.)及一個保護柱 (C18, 5μm, 4.6mm × 7.5 mm), 30°C |
| 流動相 |
1% 乙酸水溶液 : 甲醇 = 40 : 60, 1 mL/min |
| 檢測器 |
UV λ280 nm. Applied Biosystems/PESCIEX API 365 LC-MS 系統包括電噴霧電離源 (Applied Biosystems, Foster City, CA, U.S.A.). 乾燥氣: 7 L/min 300°C, 掃描範圍: 50-500 u, 孔: 26V, 聚焦: 170V, 電噴霧: 5000V. |
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| 樣品製備 |
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方法一 |
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HSCCC 儀 (Beijing Institute of New Technology Application, Beijing, China) 包括 Model GS-20 A 分析多層螺旋星式離心機及 PTFE 多層線圈70 m × 0.85 mm I.D., 總容量40 mL |
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正己烷: 乙酸乙酯: 甲醇: 水: 乙腈 = 8: 2: 5: 5: 5, v/v |
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1.0 mL/min, 1600 rpm |
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UV λ254 nm |
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方法二 |
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樣品粉末用 95% 乙醇室溫超聲提取 30 min. 以 n-C6H14, EtOAc 和 n-BuOH 分餾. |
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EtOAc 部過矽膠柱, 以100% EtOAc, EtOAc 和 CH3OH (8: 2), EtOAc 和CH3OH (1: 2), CH3OH 100% 洗脫. EtOAc 100% 餾分中得目標化合物. |
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| 參考文獻 |
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[1]
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Or, T. C. T., et al. (2011). "Isolation and identification of anti-inflammatory constituents from Ligusticum chuanxiong and their underlying mechanisms of action on microglia." Neuropharmacology 60(6): 823-831. |
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[2]
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Liu, L., et al. (2005). "Phthalide lactones from Ligusticum chuanxiong inhibit lipopolysaccharide-induced TNF-α production and TNF-α-mediated NF-κB activation." Planta Med. 71(9): 808-813. |
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[3]
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Chan, S. S.-K., et al. (2007). "Relaxation effects of ligustilide and senkyunolide A, two main constituents of Ligusticum chuanxiong, in rat isolated aorta." Journal of Ethnopharmacology 111(3): 677-680. |
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[4]
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Yi, T., et al. (2005). "Identification and comparative determination of senkyunolide A in traditional chinese medicinal plants Ligusticum chuanxiong and Angelica sinensis by HPLC coupled with DAD and ESI-MS." Chem. Pharm. Bull. 53(11): 1480-1483. |
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[5]
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Dong, J., et al. (2013). "Qualitative and quantitative analysis of the major constituents in Chinese medicinal preparation Dan-Lou tablet by ultra high performance liquid chromatography/diode-array detector/quadrupole time-of-flight tandem mass spectrometry." Journal of Pharmaceutical and Biomedical Analysis 80(0): 50-62. |
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[6]
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Wei, Y., et al. (2013). "Online isolation and purification of four phthalide compounds from Chuanxiong rhizoma using high-speed counter-current chromatography coupled with semi-preparative liquid chromatography." Journal of Chromatography A 1284(0): 53-58. |
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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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