College of Pharmaceutical Sciences, Zhejiang University, Hangzhou, PR China.
J Sep Sci. 2010 Apr;33(8):1072-8. doi: 10.1002/jssc.200900768.
An ultra-performance LC in combination with MS/MS method was established to evaluate the quality of wu-yao (the dried root of Lindera aggregata (Sims) Kosterm. (Lauraceae)) through simultaneous quantitation of five sesquiterpene lactones, linderagalactone D (1), linderagalactone C (2), hydroylindestenolide (3), neolinderalactone (4) and linderane (5). All compounds were separated on a Waters Acquity ultra-performance LC HSS T3 column (2.1 mm x 100 mm, 1.8 microm particle size) with linear gradient elution of acetonitrile and 0.1% formic acid. An ESI interface in the positive mode was employed prior to MS detection. All the compounds showed good linearity (R(2) > or = 0.9992). The recoveries, measured at three concentration levels, varied from 97.3 to 103.4% with RSDs < 4.8%. The simple, rapid and reliable method was successfully applied to quantify the five components in 13 samples of wu-yao from different areas.
建立了超高效液相色谱与串联质谱联用方法,用于通过同时定量五种倍半萜内酯(即乌药(Lindera aggregata(Sims)Kosterm.(樟科)的干燥根)的质量)。所用方法为:在 Waters Acquity UPLC HSS T3 柱(2.1mm×100mm,1.8μm 粒径)上进行线性梯度洗脱,流动相为乙腈和 0.1%甲酸;质谱检测采用正离子模式电喷雾接口。所有化合物均呈现出良好的线性(R²≥0.9992)。在三个浓度水平下进行的回收率测定结果表明,其变化范围为 97.3%至 103.4%,相对标准偏差(RSD)小于 4.8%。该简单、快速和可靠的方法成功地应用于定量分析来自不同地区的 13 个乌药样品中的这五种成分。