|
植物来源 |
|
|
生物活性 |
|
|
鉴定 |
熔点 |
38°C |
| 旋亮度 |
[α]D+40 (c, 10 氯仿) |
1HNMR
|
| 分析方法 |
|
| 仪器 |
硅胶G 板 |
| 流动相 |
乙酸乙酯: 60-90, 石油醚 = 1: 50 (v/v), 己烷: 乙酸乙酯 = 4: 1 (v/v) (展开两次) |
| 检测器 |
可见光和UV λ365 nm; 乙醇: 98% 硫酸 (9: 1, v/v) |
|
|
|
| 仪器 |
L-2130 Hitachi HPLC仪 及L-2420 Hitachi UV 检测器 |
| 色谱柱 |
Hypersil ODS-2 色谱柱 (250 mm × 4.6 nm, 5 µm) |
| 流动相 |
A: 乙腈-水, B: 水, A: B = 60: 40, 0-30 min 40-10% B, 30-40 min 10% B, 1.0 mL/min |
| 检测器 |
UV λ200 nm |
|
|
|
| 仪器 |
GC-MS仪 (GCMS-QP2010 Shimadzu) |
| 色谱柱 |
DB-5MS 毛细管柱 (30 m 60.32 mm i.d., 膜厚度0.25 lm, Agilent Technologies, USA), 温度: 280°C |
| 流动相 |
初始烘箱温度: 60°C, 2 min, 5°C/min 升至 280°C, 保持温度 6 min, 载气: 氦气, 2.0 mL/min, GC-MS 利用脉冲分流 (SCAN) 或无分流 (SIM) 注射模式, 分流比 30: 1. |
| 检测器 |
四级滤质器源及电极: 200°C ; 电子碰撞电离模式 (EI): 70 eV. 质谱全扫描模式记录 40-500 amu 全离子电流 (TIC). 对比 NIST 质谱数据库 (Shimadzu) 得到挥发油成分质谱数据. 对比文献中记载的碎片和保留时间指数鉴定质谱. |
|
|
|
| 仪器 |
GC-MS: Shimadzu GC-2010 气相色谱仪及 Shimadzu 2010 质谱; SPME 聚二甲硅氧烷 (PDMS, 100 µm) 保持器及纤维, 聚二甲硅氧烷-二乙烯基苯 (PDMS-DVB, 65 µm) 及 Stableflex 聚乙二醇-二乙烯苯 (CW-DVB, 70 µm) Supelco, USA |
| 色谱柱 |
30 m × 0.25 mm i.d. 毛细管柱, 0.25 µm 二甲基聚硅氧烷膜涂层, 60°C 解吸 5 min, 蔓延至 4°C/min 250°C, 保持 5 min |
| 流动相 |
载气: 氦气, 0.9 mL/min |
| 检测器 |
离子碰撞 (EI) 模式, 扫描范围: 40-400 amu, 离子化能: 70 eV, 扫描速率: 0.2 s/scan, 转变温度: 280°C, 离子源温度: 230°C |
|
| 样品制备 |
|
方法一 |
|
|
打粉以乙酸乙酯提取三次. 合并提取物, 45°C 减压旋转蒸发溶剂. 乙醇中溶解提取物并 -48°C 冰冻 24 小时. 分离并去除沉淀. 溶于乙酸乙酯, 分八次加入石油醚 (60-90°C) 析出沉淀. 去除杂质得初样品. |
|
|
TBE-1000A HSCCC 仪 (Tauto Biotech, Shanghai, China) 配备一个 1000 mL PTFE 盘旋柱 (1.8 mm) 及一个 100 mL 样品回路及 SD-9002 恒定流量泵, HX-2050 水浴, Model 8823B UV 检测器, 254 nm, Model N2010 色谱工作站 |
|
|
下相为石油醚 (60-90°C)-乙酸乙酯-乙醇-水 (4: 1: 4: 1, v/v) |
|
|
5.0 mL/min; 450 rpm |
|
|
UV λ254 nm |
|
|
| 参考文献 |
|
[1]
|
Shou, D., et al. (2010). Method for identifying Atractylodes macrocephala through thin-layer chromatography, Zhejiang Academy of Traditional Chinese Medicine, Peop. Rep. China. 9pp. |
|
[2]
|
Zhou, J., et al. (2012). "Comparison of the volatile compounds of crude and processed Atractylodis rhizome analyzed by GC-MS." Afr. J. Pharm. Pharmacol. 6(28): 2155-2160. |
|
[3]
|
Shi, S.-j., et al. (2012). "Effective component selection of Atractylodes extract against influenza virus." Shizhen Guoyi Guoyao 23(3): 565-566. |
|
[4]
|
D. Lorimer, S. and R. T. Weavers (1987). "Foliage sesquiterpenes and diterpenes of Podocarpus spicatus." Phytochemistry 26(12): 3207-3215. |
|
[5]
|
Wang, C.-C., et al. (2006). "Pro-oxidant and cytotoxic activities of atractylenolide I in human promyeloleukemic HL-60 cells." Food and Chemical Toxicology 44(8): 1308-1315. |
|
[6]
|
Choi, K. H., et al. (2011). "Acetylene compound isolated from Atractylodes japonica stimulates the contractility of rat distal colon via inhibiting the nitrergic-purinergic relaxation." Journal of Ethnopharmacology 134(1): 104-110. |
|
[7]
|
Kiso, Y., et al. (1985). "Mechanism of antihepatotoxic activity of atractylon, I: effect on free radical generation and lipid peroxidation." Planta Medica NO. 2: 97-100. |
|
[8]
|
Satoh, K., et al. (1996). "Specific inhibition of Na+, K+-ATPase activity by atractylon, a major component of Byaku-jutsu, by interaction with enzyme in the E2 state." Biochemical Pharmacology 51(3): 339-343. |
|
[9]
|
Shou, D., et al. (2010). Method for identifying Atractylodes macrocephala through thin-layer chromatography, Zhejiang Academy of Traditional Chinese Medicine, Peop. Rep. China. 9pp. |
|
[10]
|
Yan, K.-l., et al. (2010). "HPLC determination of atractylon, β-eudesmol and β-elemene in volatile oil of Atractylodes macrocephala Koidz." Zhongguo Yaowu Yu Linchuang 10(7): 751-753. |
|
[11]
|
Chen, Q., et al. (2009). "Identification of volatile compounds of Atractylode lancea Rhizoma using supercritical fluid extraction and GC-MS." J Sep Sci 32(18): 3152-3156. |
|
[12]
|
Guo, F.-Q., et al. (2006). "Comparison of the volatile compounds of Atractylodes medicinal plants by headspace solid-phase microextraction-gas chromatography-mass spectrometry." Analytica Chimica Acta 570(1): 73-78. |
|
[13]
|
Zhao, C. and C. He (2006). "Preparative isolation and purification of atractylon and atractylenolide III from the Chinese medicinal plant Atractylodes macrocephala by high-speed counter-current chromatography." Journal of Separation Science 29(11): 1630-1636. |
|
| 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
|
