化学名称 海帕乌头碱
外观 甲醇中呈棱晶
化学物质登录号 6900-87-4
分子式
分子量 615.71
植物来源
生物活性
鉴定 熔点 198°C
旋亮度 [α]17D+22.4 (氯仿)
UV
IR
ESI-MS
1HNMR
13CNMR
分析方法
仪器 硅胶GF254
流动相 环己烷-乙酸乙酯-二乙胺 (8: 1: 1)
检测器 Shimazu TLC model 910 仪反射膜式扫描 lambda s 236 nm 及lambda R 350 nm
仪器 Agilent 1100 series LC 系统 (Hewlett-Packard, CA, USA) 包括G1311A 四元泵, G1322A 脱气机, G1315A二极管数组检测器和G1313A 自动进样旗
色谱柱 Alltima™ RP18 色谱柱 (250 mm × 4.6 mm I.D.; 粒径5 µm; Alltech Associates, USA) Alltima™ RP18保护柱 (7.5 mm × 4.6 mm I.D.), 室温
流动相 A: 乙腈 (ACN), B: 缓冲液 (10 mM 重碳酸铵, 28% 氨溶液pH 10.0 ± 0.2), 0-10 min, 20-25% A, 10-30 min 25-34% A, 30-67 min 34-45% A, 67-75 min 45-60% A, 1.0 mL/min
检测器 UV λ240 nm
仪器 Surveyor 液相色谱 (Thermo Finnigan Corporation, San Jose, CA, USA) 配备两个溶剂泵
色谱柱 Gemini C18 色谱柱 (3 µm, 150 mm × 2 mm) (Phenomenex, Torrance, CA, USA), 包括 Phenomenex Luna 保护柱 C18 (5 µm, 4 mm × 2.0 mm i.d.), 0-3 min 20-25% B, 3-10min 25-28% B.
流动相 A 相为水和 0.005% TFA (v/v); B 相为 ACN 和 0.005% TFA (v/v). 流动相过过滤器 (0.45 µm) 和脱气机, 0.1 mL/min
检测器 VWD 1100 UV 检测器 (Agilent Technologies, Waldbronn, Germany). 四极杆离子阱及 ESI 离子源 (LCQ™, Thermo Finnigan Corporation, San Jose, CA, USA). 氦气. 正离子模式, 1.35 l/min; 4.5 kV; 175°C ; 44 V; 管镜头偏移量, 0 V; 第一加倍器偏移量, −5.00 V; 第二加倍器偏移量, −6.50 V; 多级透镜间电压, −18.00 V. 双碎片: IS 检测器 (0-7.5 min); 三个生物碱测量值 (7.5-12 min). CRM 模式选择正离子分子离子 ([M+H]+)
样品制备
方法一
0.5 g 样品, 1.0 g 碱性氧化铝和 0.5 mL pH = 12 水, 以 28% 氨溶液调节为同质的混合物至于臼中以玛瑙杵混合. 上硅胶柱洗脱, 乙腈: 水 = 80: 20 v/v ph = 12. 10 mL 洗脱物稀释至 25 mL 幷 0.22 µm PTFE 膜过滤
参考文献
[1] Chen, J.-H., et al. (2008). "Determination of aconitine-type alkaloids as markers in fuzi (Aconitum carmichaeli) by LC-ESI-MS3." Journal of Pharmaceutical and Biomedical Analysis 48(4): 1105-1111.
[2] Li, M., et al. (2013). "The anti-arthritic effects of Aconitum vilmorinianum, a folk herbal medicine in Southwestern China." Journal of Ethnopharmacology 147(1): 122-127.
[3] Wang, Q., et al. (2013). "Naturally derived anti-inflammatory compounds from Chinese medicinal plants." Journal of Ethnopharmacology 146(1): 9-39.
[4] Zyuz'kov, G. N., et al. (2013). "Medication with wound-healing activity, FGBU "Nauchno-Issledovatel'skii Institut Farmakologii" Sibirskogo Otdeleniya RAMN, Russia. 7pp.
[5] Ye, L., et al. (2013). "The role of efflux transporters on the transport of highly toxic aconitine, mesaconitine, hypaconitine, and their hydrolysates, as determined in cultured Caco-2 and transfected MDCKII cells." Toxicol Lett 216(2-3): 86-99.
[6] Wang K.; Tong Y.Y., 1990: "Determination of the main alkaloids in wu tou aconite by tlc densitometry." Yaoxue Xuebao. 25(5): 387-390
[7] Xie, Y., et al. (2005). "Simultaneous determination of six Aconitum alkaloids in proprietary Chinese medicines by high-performance liquid chromatography." Journal of Chromatography A 1093(1-2): 195-203.
[8] WEI Wei, LI Xu-wen, SHI Xiao-lei, ZHOU Hong-yu, YANG Rui-jie, ZHANG Han-qi and JIN Yong-ri*, "Matrix Solid-phase Dispersion Extraction of Alkaloids from the Roots of Aconitum kusnezoffii Reichb." College of Chemistry, Jilin University, Changchun 130012, P. R. China
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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