化学名称 淫羊藿苷
外观 黄色针晶 (吡啶溶液)
化学物质登录号 489-32-7
分子式
分子量 676.67
植物来源
生物活性
鉴定 熔点 231-235°C (226-229°C)
旋亮度 [α]15D-87.1° (Py)
1HNMR
13CNMR
分析方法
仪器 硅胶H 板
流动相 氯仿: 甲醇: 甲酸 = 15: 1: 0.2, v/v
检测器 5% 三氯化铁的乙酸喷淋显色
仪器 LC-10ATVP HPLC 泵, Shimadzu, Japan
色谱柱 ODS 色谱柱 (Shim-pack VP-ODS 4.6 mm × 150 mm, 5.0 μm, Dikma, Beijing)
流动相 乙腈: 3% 乙酸 = 29: 71, v: v, 1.0, 1.1 和1.0 mL/min
检测器 UV λ270 nm
仪器 Waters Acquity™ 仪包括二极管数组检测器 (DAD)
色谱柱 Acquity UPLC BEH C18 色谱柱 (50 mm × 2.1 mm i.d., 1.7 mm; Waters, Milford, MA, USA)
流动相 A: 100% 缓冲液 = 2.5 mM NH4Ac, pH 7.4, B: 100% 乙腈, 0.45 mL/min
检测器 UV λ254 nm
仪器 The Agilent G6410A 三重四极杆串联液相色谱-质谱系统
色谱柱 ZORBAX SB-C18 色谱柱 (3.5 μm, 2.1 mm × 100 mm) 和 C18 保护柱 (5 μm, 4.0 mm × 2.0 mm), 35°C
流动相 乙腈: 水: 甲酸 = 50: 50: 0.05, v/v/v, 0.25 mL/min
检测器 正离子模式, 4000 V, 雾化气 40 psi, 10 L/min
样品制备
方法一
两相溶剂系统正己烷-正丁醇-甲醇-水 (1: 4: 2: 6, v/v). 两个多层螺旋星式离心. 300 mg 提取物利用半制备仪器分离 230-ml 色谱柱分离103 mg 淫羊藿苷, 纯度 86.2%.
8 g 提取物利用大型制备仪器分离 2460-ml 色谱柱分离 2.45 g 淫羊藿苷纯度 85.7%. 馏分中 98% 纯淫羊藿苷水中重结晶备用.
参考文献
[1] Yang, L., et al. (2013). "Icariin from Epimedium brevicornum Maxim promotes the biosynthesis of estrogen by aromatase (CYP19)." Journal of Ethnopharmacology 145(3): 715-721.
[2] Hsieh, T.-P., et al. (2010). "Icariin isolated from Epimedium pubescens regulates osteoblasts anabolism through BMP-2, SMAD4, and Cbfa1 expression." Phytomedicine 17(6): 414-423.
[3] Li, H.-f., et al. (2012). "Antioxidant flavonoids from Epimedium wushanense." Fitoterapia 83(1): 44-48.
[4] Zhang, D. W., et al. (2008). "Effects of total flavonoids and flavonol glycosides from Epimedium koreanum Nakai on the proliferation and differentiation of primary osteoblasts." Phytomedicine 15(1–2): 55-61.
[5] Wang, L., et al. (2009). "Icariin enhances neuronal survival after oxygen and glucose deprivation by increasing SIRT1." European Journal of Pharmacology 609(1–3): 40-44.
[6] Wang, F., et al. (2012). "Icariin enhances the healing of rapid palatal expansion induced root resorption in rats." Phytomedicine 19(11): 1035-1041.
[7] Zhu, J., et al. (2008). "TLC identification for four medicinal materials and the determination of icariin in Tianshenyizhi capsule." Shizhen Guoyi Guoyao 19(2): 324-326.
[8] Li, Y., et al. (2009). "In vivo pharmacokinetics comparisons of icariin, emodin and psoralen from Gan-kang granules and extracts of Herba Epimedii, Nepal dock root, Ficus hirta yahl." Journal of Ethnopharmacology 124(3): 522-529.
[9] Liu, W., et al. (2011). "Sensitive and robust UPLC–MS/MS method to determine the gender-dependent pharmacokinetics in rats of emodin and its glucuronide." Journal of Pharmaceutical and Biomedical Analysis 54(5): 1157-1162.
[10] Xu, W., et al. (2007). "LC–MS/MS method for the simultaneous determination of icariin and its major metabolites in rat plasma." Journal of Pharmaceutical and Biomedical Analysis 45(4): 667-672.
[11] Du, Q., et al. (2002). "Purification of icariin from the extract of Epimedium segittatum using high-speed counter-current chromatography." Journal of Chromatography A 962(1–2): 239-241.
连结 中药材图像数据库 药用植物图像数据库 中药标本数据库

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