化學名稱 甘草黃苷
外觀 白色至淡黃色粉末
化學物質登錄號 551-15-5
分子式
分子量 418.39
植物來源
生物活性
鑑定 熔點 212°C
1HNMR
13CNMR
分析方法
儀器 矽膠G板
流動相 氯仿: 甲醇: 水 = 45: 17: 5, v/v/v
檢測器 UV365 nm
儀器 LC-10ATVP HPLC 泵 (Shimazdu, Japan) 配備 SPD-10AVP UV檢測器 (Shimazdu, Japan)
色譜柱 Diamonsil-C18 色譜柱 250 mm × 4.6 mm I.D. (5 µm C18 矽膠, Dikma Company, Beijing, China)
流動相 冰醋酸: 水: 乙腈 = 2.3 : 75.7: 22 (v/v/v); 流速: 1.0 mL/min
檢測器 UV λ276 nm
儀器 HP1100 色譜儀 Agilent Technologies, USA
色譜柱 C18 色譜柱 (250 mm × 4.6 mm × 5 µm, Agilent Technologies, USA)
流動相 A: 乙腈, B: 0.5% 乙酸溶液, 0-11 min 20-40% B, 11-19 min 40% B, 19-20 min 40-20% B; 流速: 1.0 mL/min.
檢測器 UV λ276 nm
儀器 Agilent 1200LC 色譜儀, U.S.A.
色譜柱 ODS 色譜柱 (250 mm × 4.6 mm, 5 µm, Agilent, U.S.A.), 25°C
流動相 甲醇: 水 = 45: 55, v/v; 1.0 mL/min
檢測器 UV λ276 nm
儀器 Hewlett-Packard (Waldbronn, Germany) 系統配備 HP1100 series 二元泵, HP1100 series 光電二極管數組檢測器和 HP1100 series 自動進樣器 (5 µl)
色譜柱 Wako Wakosil-II 5C18 AR 反相色譜柱 (粒徑5 µm, 150 × 4.6 mm i.d.)
流動相 0.01% (v/v) 硫酸: 乙腈 = 0 min, 90: 10; 10 min, 88: 12; 22 min, 70: 30; 30 min, 30: 70; 流速: 1.0 mL/min
檢測器 UV λ245 nm
儀器 Waters HPLC 系統包括一個泵 (Model 1525), 自動進樣器 (Model 717 plus), UV檢測器 (Waters 2487 Dual λ 吸收光譜檢測器)
色譜柱 Kromasil-C18 色譜柱 (5 µm, 4.6 × 250 mm, Akzol Nobel, Sweden)
流動相 甲醇: 水: 乙酸 = 65: 35: 2, v/v/v; 流速: 1.0 mL/min
檢測器 UV λ246 nm
樣品製備
方法一
150.0 mg PVPB 置入空的聚丙烯墨盒 (Alltech, Deerfield, IL, USA) 預先準備乙醇. 乾燥, 打粉, 1.0 g 樣品用 25.0 mL 甲醇提取 4 小時. SPE 墨盒上樣 0.2 mL. 3.0 mL 乙腈和甲醇: 水沖洗 (75: 25, v/v). 甲醇和甲醇: 乙酸 (90: 10, v/v) 洗脫.
方法二
1000 g 樣品用去離子水回流提取 (3 × 3 L) 重複三次 (1 hr). 合併, 真空濃縮得 340 g 提取物, 過大孔吸附樹脂 D101 柱 (10 × 80 cm, Naikai Chemical Co., China), 洗脫, 去離子水 (1 L), 50% 乙醇 (3 L), 95% 乙醇 (3 L) 得三個餾分: 水餾分 (AE1, 122 g), 50% 乙醇餾分 (AE2, 26.8 g), 95% 乙醇餾分 (AE3, 8.83 g). AE2 過矽膠柱 (500 g, 5 × 50 cm, 200 mesh, Qingdao Haiyang Chemical Co., China), 氯仿-MeOH 洗脫 (4: 1, 3: 1, 2: 1, 1: 1, 300 ml), 得到 4 餾分 (sfr): sfr.1 至 sfr.4. 分餾分 3 過 ODS 矽膠柱 (1 × 30 cm, 100 mesh, Fuji Silysia Chemical Ltd. Japan), 洗脫 MeOH- 水, 10% 至 70%, 10% 增量, 每次100 ml. 30% MeOH 洗脫物中得目標化合物 (289 mg)
參考文獻
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[2] Ammar, N. M., et al. (2012). "Phytochemical and clinical studies of the bioactive extract of Glycyrrhiza glabra L. Family Leguminosae." Int. J. Phytomed. 4(3): 429-436, 428pp.
[3] Zhao, Z., et al. (2008). "Antidepressant-like effect of liquiritin from Glycyrrhiza uralensis in chronic variable stress induced depression model rats." Behavioural Brain Research 194(1): 108-113.
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[5] Zhu, X., et al. (2006). Xuefuzhuyu capsules containing Chinese medicines and its quality control, Tianjin Hongrentang Pharmaceutical Co., Ltd., Peop. Rep. China. 25pp.
[6] Cong, J. and B. Lin (2007). "Separation of Liquiritin by simulated moving bed chromatography." Journal of Chromatography A 1145(1-2): 190-194.
[7] Sun, C., et al. (2007). "Separation of glycyrrhizic acid and liquiritin from licorice root by aqueous nonionic surfactant mediated extraction." Colloids and Surfaces A: Physicochemical and Engineering Aspects 305(1-3): 42-47.
[8] Wang, S., et al. (2013). "Facile optimization for chromatographic separation of liquiritin and liquiritigenin." Journal of Chromatography A 1282(0): 167-171.
[9] Okamura, N., et al. (1999). "Simultaneous high-performance liquid chromatographic determination of puerarin, daidzin, paeoniflorin, liquiritin, cinnamic acid, cinnamaldehyde and glycyrrhizin in Kampo medicines." Journal of Pharmaceutical and Biomedical Analysis 19(3-4): 603-612.
[10] Yang, L., et al. (2013). "Development of sample preparation method for isoliquiritigenin, liquiritin, and glycyrrhizic acid analysis in licorice by ionic liquids-ultrasound based extraction and high-performance liquid chromatography detection." Food Chemistry 138(1): 173-179.
[11] Bi, W., et al. (2010). "Solid-phase extraction of liquiritin and glycyrrhizin from licorice using porous alkyl-pyridinium polymer sorbent." Phytochemical Analysis 21(5): 496-501.
連結 中藥材圖像數據庫 藥用植物圖像數據庫 中藥標本數據庫

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