Pharmaceutical Research and Technology Institute, Kinki University, 3-4-1 Kowakae, Higashi-osaka, Osaka 577-8502, Japan.
J Pharm Biomed Anal. 2010 Sep 5;52(5):770-3. doi: 10.1016/j.jpba.2010.02.025. Epub 2010 Feb 25.
A practical HPLC-MS method for the quantitative determination of salacinol (1) and kotalanol (2), potent alpha-glucosidase inhibitors from Salacia species (Hippocrateaceae) as a specific remedy for diabetes in Ayurvedic system, was developed. The optimum conditions of separation and detection of these two constituents were achieved on a Asahipak NH2P-50 column (5 mcirom particle size, 2.0 mm i.d. x 150 mm) with a CH(3)CN-H(2)O mobile phase, associated with MS using electrospray ionization source. The overall recoveries of 1 (85.8-112.6%) and 2 (99.7-106.1%), and relative standard deviation values of intra- and inter-day precision were lower than 6.8 and 8.5%, respectively. The detection (S/N=3) and quantitation limits (S/N=10) were established to be 0.015 and 0.050 ng for 1, and 0.030 and 0.10 ng for 2, respectively. The correlation coefficients of all the calibration curves showed good linearity within test ranges. The extraction process was also optimized as 2 h immersion in water under reflux. The method was applied to evaluate extracts of three kinds of Salacia species, i.e. S. reticulata, S. oblonga, and S. chinensis, and those of four different parts, i.e. roots, stems, leaves and fruits of the same material, revealing that the extract from the roots of S. reticulata had the highest contents of these compounds. The results indicated that the assay was reproducible and precise and could be readily utilized for the evaluation of Salacia species.
建立了一种实用的 HPLC-MS 方法，用于定量测定 Salacia 属（藤黄科）中具有强α-葡萄糖苷酶抑制活性的化合物 salacinol（1）和 kotalanol（2），这些化合物是 Ayurvedic 系统治疗糖尿病的特定药物。在 Asahipak NH2P-50 柱（5 µm 粒径，2.0 mm id x 150 mm）上，采用 CH(3)CN-H(2)O 流动相，并结合电喷雾电离源的 MS，实现了这两种成分的最佳分离和检测条件。1（85.8-112.6%）和 2（99.7-106.1%）的总回收率，以及日内和日间精密度的相对标准偏差值均低于 6.8%和 8.5%。检测限（S/N=3）和定量限（S/N=10）分别确定为 1 为 0.015 和 0.050 ng，2 为 0.030 和 0.10 ng。所有校准曲线的相关系数均表现出良好的线性关系。提取过程也优化为在回流下水浸泡 2 小时。该方法应用于评价三种 Salacia 属植物，即 S. reticulata、S. oblonga 和 S. chinensis，以及同一材料的四个不同部位，即根、茎、叶和果实的提取物，结果表明来自 S. reticulata 的根提取物中这些化合物的含量最高。结果表明，该测定方法具有重现性和精确性，可用于评价 Salacia 属植物。
