Kawahara Yuki, Hoshino Tatsuro, Morimoto Hidetaka, Shinizu Tomofumi, Narukawa Yuji, Fuchino Hiroyuki, Kawahara Nobuo, Kiuchi Fumiyuki
Faculty of Pharmacy, Keio University, 1-5-30 Shibakoen, Minato-ku, Tokyo, 105-8512, Japan.
Research Center for Medicinal Plant Resources, National Institute of Biomedical Innovation, Health and Nutrition, 1-2 Hachimandai, Tsukuba, Ibaragi, 305-0843, Japan.
J Nat Med. 2016 Jan;70(1):102-6. doi: 10.1007/s11418-015-0942-4. Epub 2015 Oct 6.
A liquid chromatography mass spectrometry (LC-MS) method was developed for simultaneous quantitative analysis of Achyranthes root saponins: chikusetsusaponins IVa (1) and V (2), achyranthosides B (3), C (4), D (5), E (6), and G (7), sulfachyranthosides B (8) and D (9), and betavulgarosides II (10) and IV (11). Satisfactory separation of the saponins was achieved with the use of a volatile ion-pair reagent (dihexyl ammonium acetate) on a phenyl-hexylated silica gel column, and the amounts of saponins extracted under three different conditions were determined. When Achyranthes root was extracted with water at room temperature, achyranthosides B (3) and D (5) were the major saponins, and smaller amounts of other saponins (4, 6-11) were present. However, the amounts of chikusetsusaponins (1 and 2) were negligible. Under the condition to make a standard decoction of a Kampo formula, the major saponins were achyranthosides B (3), C (4), and D (5), and small amounts of chikusetsusaponins IVa (1) and V (2) appeared, whereas prolonged heating largely increased the amounts of chikusetsusaponins. This method can be used for quality control of Achyranthes root.
建立了一种液相色谱-质谱联用（LC-MS）方法，用于同时定量分析牛膝皂苷：牛膝皂苷IVa（1）和V（2）、牛膝甾酮苷B（3）、C（4）、D（5）、E（6）和G（7）、磺基牛膝甾酮苷B（8）和D（9）以及β-香豆素苷II（10）和IV（11）。使用挥发性离子对试剂（乙酸二己基铵）在苯基己基化硅胶柱上实现了皂苷的满意分离，并测定了在三种不同条件下提取的皂苷量。当牛膝在室温下用水提取时，牛膝甾酮苷B（3）和D（5）是主要皂苷，其他皂苷（4、6-11）含量较少。然而，牛膝皂苷（1和2）的含量可忽略不计。在制备汉方配方标准汤剂的条件下，主要皂苷为牛膝甾酮苷B（3）、C（4）和D（5），少量牛膝皂苷IVa（1）和V（2）出现，而长时间加热大大增加了牛膝皂苷的含量。该方法可用于牛膝的质量控制。
