植物来源 |
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生物活性 |
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鉴定 |
熔点 |
337-339°C |
1HNMR
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分析方法 |
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仪器 |
HSGF254 硅胶板 (Yantai Chemical Engineering Institute, China) |
流动相 |
甲苯: 乙酸抑制: 丙酮: 甲酸 = 20: 4: 2: 1 |
检测器 |
UV λ254 nm; 浓氨溶液烟雾显色 |
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仪器 |
Shimadzu LC-2010AHT HPLC 仪和Shimadzu CLASS-VP 软件version 6.12 SP4 (Shimadzu Co. Ltd., Japan) |
色谱柱 |
Kromasil C18 色谱柱 (4.6 × 250 mm, 5 µm, Tianjin Scientific Instruments Co. Ltd., China), 40°C |
流动相 |
A: 0.5% 冰醋酸水溶液, B: 0.5% 冰醋酸甲醇溶液, 0-10 min 30% B, 10-30 min 30-40% B, 30-40 min 40% B, 40-60 min 40-60% B, 进样量: 25 µL, 1.0 mL/min |
检测器 |
UV λ257.2 nm |
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仪器 |
Agilent 1200 反相 HPLC 仪 |
色谱柱 |
HiQ Sil C18W 反相色谱柱 (250 mm × 4.6 mm i.d., 5 µm), 30°C |
流动相 |
甲醇: 水: 甲酸 = 35: 64.935: 0.065 (v/v/v), 1 mL/min, 进样量: 10 µl |
检测器 |
UV λ260 nm |
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|
仪器 |
HP 1200 液相色谱仪, Agilent (Waldbronn, Germany), 配备一个二元泵, 膜脱气机, 自动进样器, 和六通阀. |
色谱柱 |
Zorbax Eclipse XDB-C18 色谱柱 (50 × 4.6 mm2, 1.8 µm), 25°C |
流动相 |
A: 乙腈, B: 0.01% 甲醇水, 0-1.5 min 10% A, 1.5-2.5 min 10-25% A, 2.5-3.5 min 25% A, 3.5-7 min 25-50% A, 7-8 min 50-80% A, 8-10 min 80% A, 10-12 min 80-10% A, 0.5 mL/min, 进样量: 10 µL |
检测器 |
Triple Quad LC/MS 6410 仪 (Agilent) 配备 ESI 源. ESI-MS 利用正离子多反应监视模式 (MRM), 电喷雾毛细管电压: 3500 V, 雾化气压: 35 psi. 干燥气流速: 氮气12 L/min at 350°C. Agilent Mass Hunter 软件控制, version B.04.01. |
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样品制备 |
方法一 |
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Type-J 多线圈行星离心机 (P.C. Inc., Potomac, MD, USA). 离心中心轴距离 10 cm. 单 Tefzel 管分离柱 (Zeus Industrial Products) 1.6 mm I.D. (SW 14), 长160 m, 12 层, 2 吋间距. 柱总容量 320 ml. β值内部为 0.5、外部 0.75. 转速控制器 (Bodine Electric, North Chicago, IL, USA), 800 rpm. UV 检测器 (Uvicord S, LKB Instruments, Bromma/Stockholm, Sweden). 馏分收集器 (Ultrorac, LKB Instruments). |
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下相为HCl3-MeOH-H2O (4: 3: 2, v/v) |
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2.0 mL/min; 800 rpm |
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UV λ275 nm |
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方法二 |
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负压空化装置 (CN2597047), 一个提取和一个收集罐, 氮气提取, 恒温控制, 挥发性溶剂冷凝器冷藏。 |
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10 g 样品置于负压空化装置提取, 利用真空泵减压提取。异黄酮的提取时间, 粒径, 负压, 乙醇浓度, 液固比都可被控制。 |
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参考文献 |
[1]
|
Zhang, D.-Y., et al. (2010). "Negative pressure cavitation extraction and antioxidant activity of genistein and genistin from the roots of pigeon pea [Cajanus cajan (L.) Millsp.]." Separation and Purification Technology 74(2): 261-270. |
[2]
|
Shodehinde, S. A. and G. Oboh (2013). "Antioxidant properties of aqueous extracts of unripe Musa paradisiaca on sodium nitroprusside induced lipid peroxidation in rat pancreas in vitro." Asian Pacific Journal of Tropical Biomedicine 3(6): 449-457. |
[3]
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Lee, J. H., et al. (2013). "Determination of the variations in levels of phenolic compounds in soybean (Glycine max Merr.) sprouts infected by anthracnose (Colletotrichum gloeosporioides)." J Sci Food Agric 93(12): 3081-3086. |
[4]
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Kasper, J. and M. F. Melzig (2011). "HPTLC method for the quantification of isoflavones in nutritional supplements of red clover (Trifolium pratense L.)." J. Planar Chromatogr.--Mod. TLC 24(5): 373-375. |
[5]
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Lengyel, J., et al. (2013). "On the radical scavenging activity of isoflavones: thermodynamics of O-H bond cleavage." Physical Chemistry Chemical Physics 15(26): 10895-10903. |
[6]
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Vitale, D. C., et al. (2013). "Isoflavones: estrogenic activity, biological effect and bioavailability." Eur J Drug Metab Pharmacokinet 38(1): 15-25. |
[7]
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Weng, C. J. and G. C. Yen (2012). "Flavonoids, a ubiquitous dietary phenolic subclass, exert extensive in vitro anti-invasive and in vivo anti-metastatic activities." Cancer Metastasis Rev 31(1-2): 323-351. |
[8]
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Bae, M., et al. (2012). "Inhibitory effects of isoflavonoids on rat prostate testosterone 5alpha-reductase." J Acupunct Meridian Stud 5(6): 319-322. |
[9]
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Hirohata, M., et al. (2012). "Anti-amyloidogenic effects of soybean isoflavones in vitro: Fluorescence spectroscopy demonstrating direct binding to Aβ monomers, oligomers and fibrils." Biochimica et Biophysica Acta (BBA) - Molecular Basis of Disease 1822(8): 1316-1324. |
[10]
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Masilamani, M., et al. (2012). "Regulation of the immune response by soybean isoflavones." Immunologic Research 54(1-3): 95-110. |
[11]
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Kim, J. H., et al. (2012). "A new isoflavone glycitein 7-O-beta-D-glucoside 4\'-O-methylate, isolated from Cordyceps militaris grown on germinated soybeans extract, inhibits EGF-induced mucus hypersecretion in the human lung mucoepidermoid cells." Phytother Res 26(12): 1807-1812. |
[12]
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Yuan, D., et al. (2006). "TLC and HPLC analysis of soy isoflavones in Semen Sojae Praeparatum." Asian J. Tradit. Med. 1(3-4): 166-172. |
[13]
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Delgado-Zamarreño, M. M., et al. (2012). "A modified QuEChERS method as sample treatment before the determination of isoflavones in foods by ultra-performance liquid chromatography-triple quadrupole mass spectrometry." Talanta 100(0): 320-328. |
[14]
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Yang, F., et al. (2001). "Separation and purification of isoflavones from a crude soybean extract by high-speed counter-current chromatography." Journal of Chromatography A 928(2): 163-170. |
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连结 |
中药材图像数据库
药用植物图像数据库
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