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植物來源 |
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生物活性 |
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鑑定 |
熔點 |
192-195°C |
| 旋光度 |
[α]20D-13.4 (c, 3.65 DMF) |
1HNMR
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| 分析方法 |
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| 儀器 |
矽膠板GF254 |
| 流動相 |
氯仿: 乙酸抑制: 甲醇: 濃氨 = 10: 2: 2.5: 0.5 |
| 檢測器 |
UV λ365 nm; 10% 硫酸乙醇, 加熱至105°C |
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| 儀器 |
Hewlett Packard series 1100 HPLC儀 (Hewlett Packard, palo alto, CA, USA)包括二元泵 (G1322A) 和二極管數組檢測器 (G1315A) |
| 色譜柱 |
Waters C18 色譜柱 (Hypersil ODS, 4.6 × 250 mm, 5 µM, Wexford, Ireland) |
| 流動相 |
A: 1% 乙酸水 (v/v), B: 乙腈, 0-40 min 10-20%, 40-70 min 20-100%, 0.8 mL/min |
| 檢測器 |
UV λ260 nm |
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| 儀器 |
PU-980 Intelligent HPLC 泵及DG-980-50-3-在線脫氣機, LG-980-02 三元梯度單元, MD-1510 可變波長檢測器 (Jasco, Gross-Umstadt, Germany) |
| 色譜柱 |
Luna C18 (2) 色譜柱 (Phenomenexm, Aschaffenburg, Germany, 5 µm, 250 mm × 4.6 mm 保護柱) |
| 流動相 |
A: 0.1% 甲酸, B: CAN, 0-30 min 85% A, 30-40 min 76% A, 40-45 min 10% A, 45 min 85% A, 0.8 mL/min |
| 檢測器 |
UV λ260 nm |
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| 儀器 |
UPLC™ 儀 (Waters Acquity System, Milford, MA, USA) 包括二元泵和自動進樣器和二極管數組檢測器 (Waters 2996, Milford, MA) |
| 色譜柱 |
反相Acquity UPLCTM EH C18 柱1.7 µm (2.1 × 50 mm) (Waters Corp., Milford, MA, USA), 35°C |
| 流動相 |
A: 0.1% 甲酸超純水溶液, B: 0.1% 甲酸乙腈溶液, 0-1 min 10% B, 1-3 min 12% B, 3-4 min 22% B, 4-5 min 23% B, 5-6 min 35% B, 6-8 min 50%, 8-8.1 min 50% B, 8.1 min 10% B, 0.6 mL/min |
| 檢測器 |
UV λ262 nm |
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| 儀器 |
包括兩個泵 (LC-10ADvp, Shimadzu, Toyoto, Japan), 在線脫氣機 (DGU-12A, Shi-madzu), 三重四極杆串聯質譜及 ESI 源 (TSQ Quantum, Thermo Scientific, San Jose, CA). Xcalibur 軟件 (Thermo Finnigan) 控制 |
| 色譜柱 |
反相色譜柱 (C18, 150 mm × 2.1 mm, 5 µm) |
| 流動相 |
A: 10% 乙腈/ 0.1% 甲酸, B: 90% 乙腈/ 0.1% 甲酸, 0-20 min 10-45% B; 20-25 min 100% A; 0.25 mL/min |
| 檢測器 |
MS 正離子模式檢測, 噴霧電壓: 3 kV, 氣化溫度: 300°C, 管透鏡電壓: 150 V; 毛細管電壓: 35 V, 毛細管溫度: 270°C, 鞘氣及輔助氣: 35 和10; 碰撞誘導解離 (CID): 30 V, m/z 255→199 黃豆苷元, m/z 271→153 染料木黃酮, m/z 285→242 黃豆黃素和毛蕊異黃酮 (IS), m/z 417→255 for 黃豆苷, m/z 433→271 染料木苷, m/z 447→285 黃豆黃素苷, SRM 檢測 |
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| 樣品製備 |
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方法一 |
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75% 甲醇提取. SPE 提取利用Amberlite XAD-7 (Fluka, Buchs, Switzerland) 玻璃柱 (45 cm × 65 cm). 用水沖洗, 乙醇洗脫, XAD-7 異黃酮提取物. 利用 HSCCC 以 MTBE/ ACN/ 水 (2/2/3 v/v/v) 為流動相3.2 mL/min. 600 rpm, UV λ260 nm. 得三餾分, 餾分 1 再用 HSCCC 分離, \"一步法梯度溶劑系統\" 分離大豆苷和黃豆黃苷. |
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HSCCC儀 Pharma-Tech Research (Baltimore, Maryland, USA), 3製備線圈 (總容量850 mL, id 2.6 mm), Biotronik HPLC 泵BT 3020, Knauer 可變波長檢測 |
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初始兩相溶劑系統: MTBE/正丁醇/ACN/水 (2/1/2/5 v/v/v/v), 下相為流動相; 280 min: MTBE 飽和水和 ACN (10/1 v/v) |
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2.5 mL/min; 600 rpm |
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UV λ315 nm |
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方法二 |
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0% 乙醇 60°C 提取三次. 蒸幹溶劑, 純水溶解, 氯仿 1: 1 分離兩次. 乙醇-水部分餾三次, 丁醇1: 1. 真空乾燥. |
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丁醇提取物過 Sephadex LH-20 柱 (100 M, Pharmacia Fine Chemical Co., Ltd., Germany) 70% 乙醇洗脫得 20 餾分 (F1-F20). 餾分 F7-F16 過 Sephadex LH-20 柱. 純乙醇洗脫. |
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C18 HPLC 製備色譜柱 (Hypersil ODS, 250 × 22 mm, 10 m, Alltech, Deerfield, IL, USA) 純化, 含1% 乙酸10% 乙腈洗脫純化, 蒸幹, 溶於乙醇. |
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方法三 |
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SFE 提取的樣品. 70% 乙醇水溶液回流提取. 濃縮, 去溶劑. 過 D101 大孔吸附樹脂柱. 以水和 40%, 75%, 95% 乙醇洗脫. |
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製備 HPLC (pHPLC) 分離. 系統: Waters 515 泵, 2487 檢測器, N2000 工作站 (Zhejiang University, Hangzhou, China); 色譜柱: YWG C18 (20.0 × 250 mm, i.d. 10 μm) (Hanbon Science and Technology CO., Ltd. Jiang Su province, China); 流動相: 乙腈-水-乙酸 (25: 75: 2 和 35: 65: 2 v/v/v); 流速: 3.5 和 4.5 mL/min; 檢測: 260 nm |
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| 參考文獻 |
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[1]
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Lee, C. H., et al. (2005). "Relative antioxidant activity of soybean isoflavones and their glycosides." Food Chemistry 90(4): 735-741. |
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[2]
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Shi, S., et al. (2012). "Systematic separation and purification of 18 antioxidants from Pueraria lobata flower using HSCCC target-guided by DPPH-HPLC experiment." Separation and Purification Technology 89(0): 225-233. |
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[3]
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Lapčík, O., et al. (2005). "Identification of isoflavones in Acca sellowiana and two Psidium species (Myrtaceae)." Biochemical Systematics and Ecology 33(10): 983-992. |
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[4]
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Li, X., et al. (2009). "Isoflavone glycosides from the bark of Maackia amurensis." Yaoxue Xuebao 44(1): 63-68. |
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[5]
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Pandey, A., et al. (2011). "Pharmacological screening of Coriandrum sativum Linn. for hepatoprotective activity." J Pharm Bioallied Sci 3(3): 435-441. |
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[6]
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Lee, E.-J., et al. (2010). "Glycitein inhibits glioma cell invasion through down-regulation of MMP-3 and MMP-9 gene expression." Chemico-Biological Interactions 185(1): 18-24. |
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[7]
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Roland, W. S., et al. (2011). "Soy isoflavones and other isoflavonoids activate the human bitter taste receptors hTAS2R14 and hTAS2R39." J Agric Food Chem 59(21): 11764-11771. |
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[8]
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Muñoz, Y., et al. (2009). "Equol is more active than soy isoflavone itself to compete for binding to thromboxane A2 receptor in human platelets." Thrombosis Research 123(5): 740-744. |
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[9]
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Wang, Z.-s., et al. (2012). "Study on the quality standard of peigen capsules." Zhongguo Yaofang 23(7): 635-637. |
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[10]
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Stürtz, M., et al. (2006). "Preparative isolation of isoflavones from soy and red clover." Molecular Nutrition & Food Research 50(4-5): 356-361. |
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[11]
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Toro-Funes, N., et al. (2012). "Fast simultaneous determination of free and conjugated isoflavones in soy milk by UPLC." Food Chemistry 135(4): 2832-2838. |
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[12]
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Qing, L.-S., et al. (2013). "Rapid Magnetic Solid-Phase Extraction for the Selective Determination of Isoflavones in Soymilk Using Baicalin-Functionalized Magnetic Nanoparticles." Journal of Agricultural and Food Chemistry 61(34): 8072-8078. |
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[13]
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Qu, L.-p., et al. (2007). "Isolation of six isoflavones from Semen sojae praeparatum by preparative HPLC." Fitoterapia 78(3): 200-204. |
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| 連結 |
 中藥材圖像數據庫
藥用植物圖像數據庫
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