HPLC-MS-MS同时测定山银花中10种活性成分的含量  

Simultaneous determination of ten bioactive constituents in Lonicerae Flos by HPLC-MS-MS

作　　者：王亚丹[1] 何轶[1] 戴忠[1] 马双成[1] 

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《中国中药杂志》2016年第10期1870-1875,共6页China Journal of Chinese Materia Medica

基　　金：国家自然科学基金项目(81173506);国家"重大新药创制"科技重大专项(2014ZX09304307-002)

摘　　要：该实验建立了HPLC-MS-MS方法用于同时测定山银花中6种环烯醚萜和4种黄酮类成分的含量。采用Shiseido Capcell Pak-C18色谱柱（4.6 mm×250 mm,5μm）;流动相为0.1%甲酸水溶液（A）-乙腈（B）;质谱采用ESI^-多反应监测（MRM）模式扫描。方法学验证结果显示,10个化合物在各自浓度范围内线性关系良好（R^2≥0.999 0）,定量限（LOQ）为7.4-31.0μg·L^-1,平均回收率在94.16%-105.3%。样品测定结果表明,山银花中环烯醚萜总量（0.338%-1.440%）远高于黄酮总量（0.015 4%-0.057 5%）,其中马钱素-7-酮、裂环马钱酸、马钱苷酸、裂环氧化马钱素、木犀草苷、异槲皮苷等6个单体化合物在3种植物来源的药材中含量具有显著差异,为山银花基原植物的鉴定和质量标准完善提供了科学依据。In this study,an HPLC-MS/MS method was developed and validated for simultaneous determination of six iridoids and four flavonoids in batches of Lonicerae Flos samples. Chromatographic separation was performed on a Shiseido Capcell Pak-C18column（ 4. 6 mm × 250 mm,5 μm）. 0. 1% Aqueous formic and acid（ A） and acetonitrile（ B） were adopted as mobile phase. Detection was carried out on a triple quadrupole mass spectrometer in the negative ion mode using an electrospray source. Multiple reaction monitoring（ MRM） mode was employed. The developed method showed good linearity（ R^2≥0. 999 0） for all the analytes within the test ranges and the limits of quantification（ LOQs） ranged from 7. 4 to 31. 0 μg·L^- 1. The recoveries varied between 94. 16% and 105. 3%. The quantitative data indicated that the total content of iridoids（ 0. 338%-1. 440%） was much higher than that of flavonoids（ 0. 015 4%-0. 057 5%） in all samples. Moreover,it was found that there were significant differences in the content of six compounds among the samples from three different original plants,which might provide scientific evidences for the origin identification and quality control of Lonicerae Flos.

关 键 词：山银花 HPLC-MS/MS 环烯醚萜 黄酮 含量测定 

分 类 号：R284.1[医药卫生—中药学] O657.63[医药卫生—中医学]