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植物來源 |
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生物活性 |
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鑑定 |
熔點 |
244°C |
| 旋光度 |
[α]D-100 (c, 0.5 Py) |
1HNMR
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| 分析方法 |
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| 儀器 |
製備薄層色譜玻璃板 (矽膠和指示劑, 1 mm, G 1510/LS 254; 20 × 20 cm) 矽膠60, F254; 0.5 mm |
| 流動相 |
乙酸一直: 甲醇: 水 = 100: 13.5: 10 |
| 檢測器 |
UV λ254 和365 nm |
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| 儀器 |
HPLC 系統 (2695 泵, 2996二極管數組檢測系統; Waters) |
| 色譜柱 |
ODS C18 分析柱 (4.6 × 250 mm), 30°C |
| 流動相 |
ODS C18 分析柱 (4.6 × 250 mm), 30°C |
| 檢測器 |
UV λ280 nm |
|
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|
| 儀器 |
Waters Alliance 2695 (Milford, MA, USA) HPLC 系統, 配備真空脫氣機, 二元泵, 自動進樣器, 2996光電二極體陣列檢測器 |
| 色譜柱 |
Hypersil RP-C18 分析色譜柱 (4.6 mm × 250 mm, 5 µm, Dalian, China) |
| 流動相 |
A: 0.1% 甲酸水, B: 已經, 0-5 min 10-15% B, 5-10 min 15% B, 10-16 min 15-18% B, 16-17 min 19% B, 17-25 min 19-20% B, 25-28 min 20-25% B, 28-33 min 25-30% B, 33-35 min 10-15% B; 1.0 mL/min; 進樣量: 10 µl |
| 檢測器 |
酚酸: UV λ324 nm; 黃酮: UV λ283 nm; 生物鹼 UV λ273 nm; 微團 ZQ 2000 質譜包括 ESI 探針, 105°C, 黃酮和生物鹼正離子模式, 酚酸用負離子模式, 去溶劑氣: 氮氣, 250 L/h, 250°C, 毛細管和錐電壓: 3500 和40 V, ESI+, 3000 和25 V, ESI- |
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| 儀器 |
ACQUITY UPLC 系統 (Waters Corp., Milford, MA, USA) 包括一個二元泵, 一個自動進樣器, 一個高溫柱溫箱 (HT) |
| 色譜柱 |
ACQUITY UPLC HSS T3 C18 色譜柱 (100 mm × 2.1 mm i.d., 1.7 µm), 45°C |
| 流動相 |
A: 0.1% 甲酸水, B: 0.1% 甲酸乙腈. 0-1 min 等度1% B, 1-10 min 1-50% B, 10-12 min 50-90% B, 12-13 min 等度90% B, 13-17 min 1% B; 0.45 mL/min; 進樣量: 6 µL |
| 檢測器 |
SYNAPT G2-S 高分辨質譜 (Waters Corp., Milford, MA, USA) 包括 ESI 源, 負離子模式, 源溫度: 120°C, 去溶劑氣流: 800 L/h, 溫度: 450°C, 錐氣: 20 L/h, 樣品錐氣: 30.0 V, 提取錐氣: 4.0 V, 毛細管電壓: 2500 V, TOF 採集速率: 0.2 s/scan, 0.01 s 見掃描延遲 |
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| 樣品製備 |
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方法一 |
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80% 乙醇 2000 m1 超聲提取樣品40 min. 提取兩次. 合幷, 4000 rpm 離心 20 min. 合幷, 50°C 蒸幹. 2000 ml ddH2O 溶解粗提物. 過 D101 大孔吸附樹脂 (16 × 200 mm). BV: 20 ml; 2 mL/min. 4 BV ddH2O 沖洗去雜質. 乙醇梯度洗脫 (10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 4 BV). 收集, HPLC 分析. 50°C 真空蒸幹. HSCCC 純化粗提物 (RCE). |
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HSCCC 儀 (TBE-300A, Shanghai Tauto Biotech. Co., Ltd, China) 包括 ÄKTA FPLC™ (GE Healthcare Life Sciences) |
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20 mL/min; 800 rpm; 下相: 2 mL/min |
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UV λ280 nm |
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方法二 |
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樣品中加入含抗壞血酸的純乙醇, 攪拌幷 15000 r.p.m 離心, 去上層液備用。10 mM 抗壞血酸的甲醇提取四次, Schleicher and Schuell 595 過濾器過濾。15000 r.p.m 離心, 加入0.05 M 醋酸鈉, Buchi Rotavapor (Bibby Sterilin LTD, England) 30°C 去溶劑, 收集, 備用。 |
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鞣質餾分乙酸乙酯 1: 1 (v/v) 提取三次. 30°C 真空蒸幹, 加入乙醇. 過 20 g Sephadex LH 20 柱. 95% 乙醇沖洗去雜質, 收集幷過濾, 50% 丙酮去鞣質. 30°C 蒸幹. |
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製備薄層色譜過濾餾分, 甲醇或乙醇去除其他化合物, 純化目標化合物。 |
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| 參考文獻 |
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[1]
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van der Watt, E. and J. C. Pretorius (2001). "Purification and identification of active antibacterial components in Carpobrotus edulis L." Journal of Ethnopharmacology 76(1): 87-91. |
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[2]
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Zhang, J., et al. (2012). "Purification of naringin and neohesperidin from Huyou (Citrus changshanensis) fruit and their effects on glucose consumption in human HepG2 cells." Food Chemistry 135(3): 1471-1478. |
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[3]
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Zhang, J., et al. (2012). "The influence of compatibility of traditional Chinese medicine on the pharmacokinetic of main components in Fructus Aurantii." Journal of Ethnopharmacology 144(2): 277-283. |
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[4]
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Hamdan, D., et al. (2011). "Chemical composition and biological activity of Citrus jambhiri Lush." Food Chemistry 127(2): 394-403. |
|
[5]
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Mäkynen, K., et al. (2013). "Cultivar variations in antioxidant and antihyperlipidemic properties of pomelo pulp (Citrus grandis [L.] Osbeck) in Thailand." Food Chemistry 139(1–4): 735-743. |
|
[6]
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Cao, H., et al. (2010). "Pharmacokinetics-based elucidation on disparity in clinical effectiveness between varieties of Zhi Zhu Wan, a Traditional Chinese Medical formula." Journal of Ethnopharmacology 128(3): 606-610. |
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[7]
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Zou, Z., et al. (2013). Application of neohesperidin as an antidepressive medicine, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences, Peop. Rep. China. 9pp. |
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[8]
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El-Readi, M. Z., et al. (2010). "Inhibition of P-glycoprotein activity by limonin and other secondary metabolites from Citrus species in human colon and leukaemia cell lines." European Journal of Pharmacology 626(2–3): 139-145. |
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[9]
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Salas, M. P., et al. (2011). "Antifungal activity of natural and enzymatically-modified flavonoids isolated from citrus species." Food Chemistry 124(4): 1411-1415. |
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[10]
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He, D., et al. (2011). "Simultaneous determination of flavanones, hydroxycinnamic acids and alkaloids in citrus fruits by HPLC-DAD–ESI/MS." Food Chemistry 127(2): 880-885. |
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[11]
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Wan, J.-B., et al. (2013). "Chemical differentiation of Da-Cheng-Qi-Tang, a Chinese medicine formula, prepared by traditional and modern decoction methods using UPLC-MS-based metabolomics approach." Journal of Pharmaceutical and Biomedical Analysis 83(0): 34-42. |
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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
|
