| 分析方法 |
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| 仪器 |
Perkin Elmer series 200液相色谱仪 |
| 色谱柱 |
C8 色谱柱配置 5 μm 粒径颗粒 (Spheri-5 RP-8, Brownlee, Perkin-Elmer), 25°C |
| 流动相 |
A: 乙腈: 水 = 80: 20, B: 1% 乙酸甲醇, 0-6 min 40% A 0.45 mL/min, 6-8 min 40-60% A 0.6 mL/min, 8-10.5 min 60-30% A 0.8mL/min, 10.5-15 min 30-20% A, 15-21 min 20-40% A. |
| 检测器 |
UV λ244 nm 和 UV λ276 nm, API 3000 三重四极杆仪配备涡轮增压离子喷雾接口, 负离子模式. |
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| 样品制备 |
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方法一 |
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岭南山竹子茎皮粉末由 95% EtOH 三次, 7 天, 干燥置于水中备用, 石油醚 (3L)、氯仿 (9L)、BuOH (9L) 分馏。 |
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氯仿馏分上样睢教主以石油醚: Me2CO = 7:1, 5:1, 3:1, 1:1, 0:1 洗脱得 3 馏分. 馏分 B 上样硅胶柱石油醚: Me2CO = 5:1 至 2:1 洗脱.馏分 B2 进样 Toyopearl HW-40C 柱, MeOH 洗脱. |
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RP-C18 色谱柱纯化, MeOH: 水 = 65: 35 to 9 : 1 洗脱得目标化合物. |
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方法二 |
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乙酸乙脂 (5 L) 提取三次, 浸泡过夜并搅拌, 减压蒸干。 |
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硅胶色谱柱以庚烷-乙酸乙脂 = (95:5 - 50:50) 洗脱得 12 个馏分. 馏分 VI 上样硅胶色谱柱庚烷-乙酸乙脂 = (90:10 - 75:25) 洗脱得黄色油状物, 庚烷-乙酸乙脂 = (95:5 - 50:50) 再次色谱柱分离洗脱得10 个馏分. |
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馏分VII (350 mg) 上样硅胶色谱柱庚烷-丙酮 (95: 5 to 50: 50)洗脱的 黄色油状藤黄酚 (83 mg). |
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| 参考文献 |
|
[1]
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Hamed, W., et al. (2006). "Oblongifolins A-D, polyprenylated benzoylphloroglucinol derivatives from Garcinia oblongifolia." J Nat Prod 69(5): 774-775. |
|
[2]
|
Yu, F.-s., et al. (2013). "Chemical constituents of Garcinia oblongifolia Champ." Zhongnan Yaoxue 11(4): 241-244. |
|
[3]
|
Bakana, P., et al. (1987). "Structure and chemotherapeutical activity of a polyisoprenylated benzophenone from the stem bark of Garcinia huillensis." Journal of Ethnopharmacology 21(1): 75-84.; Claeys, M.; Tott, J.; Pieters, L. A. C.; Van Hoof, L.; Tamba-Vemba; Van den Berghe, D. A.; Vlietinck, A. J. J. Ethnopharmacol. 1987, 21, 75- 84. |
|
[4]
|
Iinuma, M.; Tosa, H.; Tanaka, T.; Kanamaru, S.; Asai, F.; Kobayashi, Y.; Miyauchi, K.; Shimano, R. Biol. Pharm. Bull. 1996, 19, 311-314. |
|
[5]
|
Rama Rao, A. V., et al. (1980). "Camboginol and Cambogin." Tetrahedron Letters 21(20): 1975-1978. |
|
[6]
|
Krishnamurthy, N., et al. (1981). "On the structures of garcinol, isogarcinol and camboginol." Tetrahedron Letters 22(8): 793-796. |
|
[7]
|
Krishnamurthy, N., et al. (1982). "Crystal and molecular structure of isogarcinol." Tetrahedron Letters 23(21): 2233-2236. |
|
[8]
|
Hartati, S., et al. (2008). "A new pyrano xanthone from the stem barks of Garcinia tetrandra Pierre." J. Biol. Sci. (Faisalabad, Pak.) 8(1): 137-142. |
|
[9]
|
Hartati, S., et al. (2007). "Chemical constituents of Garcinia maingayii." Zhongguo Tianran Yaowu 5(4): 272-276. |
|
[10]
|
Soemiati, A., et al. (2006). "Garcinopicrobenzophenone, a novel polyprenylbenzophenone from the bark of Indonesian Garcinia picrorrhiza Miq." ACGC Chem. Res. Commun. 20: 1-5. |
|
[11]
|
Fuller, R. W., et al. (1999). "Guttiferone F, the First Prenylated Benzophenone from Allanblackia stuhlmannii." J. Nat. Prod. 62(1): 130-132. |
|
[12]
|
Shan, W.-G., et al. (2012). "Polyprenylated xanthones and benzophenones from the bark of Garcinia oblongifolia." Helv. Chim. Acta 95(8): 1442-1448. |
|
[13]
|
Koeberle, A., et al. (2009). "Identification of 5-lipoxygenase and microsomal prostaglandin E2 synthase-1 as functional targets of the anti-inflammatory and anti-carcinogenic garcinol." Biochem. Pharmacol. 77(9): 1513-1521. |
|
[14]
|
Tanaka, T., et al. (2000). Anticarcinogenic agents containing polyisoprenylated benzophenones, Kikkoman Corp., Japan. 6pp. |
|
[15]
|
Liao, C.-H., et al. (2005). "Effects of garcinol on free radical generation and NO production in embryonic rat cortical neurons and astrocytes." Biochem. Biophys. Res. Commun. 329(4): 1306-1314. |
|
[16]
|
Gustafson, K. R., et al. (1992). "The guttiferones, HIV-inhibitory benzophenones from Symphonia globulifera, Garcinia livingstonei, Garcinia ovalifolia and Clusia rosea." Tetrahedron 48(46): 10093-10102. |
|
[17]
|
Hutadilok-Towatana, N., et al. (2007). "Inhibition of human lipoprotein oxidation by morelloflavone and camboginol from Garcinia dulcis." Nat. Prod. Res. 21(7): 655-662. |
|
[18]
|
Kumar, S., et al. (2009). "High-performance liquid chromatography and LC-ESI-MS method for identification and quantification of two isomeric polyisoprenylated benzophenones isoxanthochymol and camboginol in different extracts of Garcinia species." Biomed Chromatogr 23(8): 888-907. |
|
[19]
|
Chattopadhyay, S. K. and S. Kumar (2007). "A rapid liquid chromatography-tandem mass spectrometry method for quantification of a biologically active molecule camboginol in the extract of Garcinia cambogia." Biomed Chromatogr 21(1): 55-66. |
|
[20]
|
Yang, H., et al. (2010). "Benzophenones and biflavonoids from Garcinia livingstonei fruits." J Agric Food Chem 58(8): 4749-4755. |
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