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LC-MS/MS同时测定蓝萼香菜中4种二萜类成分及其聚类分析

Simultaneous determination of 4 diterpenoids in Rabdosia japonica var. glaucocalyx by HPLC-ESI-MS / MS and cluster analysis

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【作者】 田婷婷马英华解伟伟靳怡然许慧君张兰桐杜英峰

【Author】 TIAN Ting-ting;MA Ying-hua;XIE Wei-wei;JIN Yi-ran;XU Hui-jun;ZHANG Lan-tong;DU Ying-feng;School of Pharmacy,Hebei Medical University;Pharmacy Dept.,The Second Hospital of Hebei Medical University;

【机构】 河北医科大学药学院药物分析教研室河北医科大学第二医院药学部

【摘要】 建立高效液相色谱串联三重四级杆质谱法(LC-MS/MS)同时测定蓝萼香茶菜中蓝萼甲素、冬凌草甲素、河北冬凌草素K和延命草醇4种二萜类有效成分的含量。采用Agilent ZORBAX SB-C18色谱柱(4.6 mm×250 mm,5μm),流动相为甲醇-水,梯度洗脱,流速0.8 m L·min-1。采用电喷雾离子源(ESI)负离子条件下检测,多反应离子监测(MRM)进行定量。结果上述4种待测成分在测定的质量浓度范围内均具有良好的线性关系(r>0.998 7);加样回收率92.40%~105.9%,精密度RSD 1.7%~6.5%。建立的HPLC-MS/MS同时测定蓝萼香茶菜中4种有效成分的定量分析方法简便、快速、准确、重复性好,可以为综合评价蓝萼香茶菜的质量提供参考,并且根据含量测定结果表明不同药用部位和不同采收期的蓝萼香茶菜质量存在一定差异,从而得出该中药材的最佳药用部位及采收期,用于指导合理的采收,以便于更好的利用植物资源。同时对所有批次药材进行聚类分析,结果表明不同产地蓝萼香茶菜药材质量也存在一定差异。

【Abstract】 A quick HPLC-ESI-MS /MS method was established for simultaneous determination of four major diterpenoids in Rabdosia japonica var. glaucocalyx,including glaucocalyxin A,oridonin,hebeirubesensin and enmenol. Analysis was performed on an Agilent ZORBAX SB-C18(4. 6 mm × 250 mm,5 μm) column eluted in a gradient program with methanol and water. The flow rate was 0. 8 m L · min- 1. Multiple reaction monitoring( MRM) scanning mode was performed in negative ion switching mode to apply for the quantitative determination. The calibration curves for the above four compounds were linear in corresponding injection amount. The average recoveries of the compounds ranged from 92. 40 % to 105. 9 %,with RSDs of 1. 7 %-6. 5 %. The method is simple,rapid,accurate with good repeatability,which can provide a reference for overcalling evaluation the quality of R. japonica var. glaucocalyx. The result of cluster analysis- showed that the quality of R. japonica glaucocalyx var. greatly varied between areas and parts.

【基金】 国家自然科学基金项目(81402894)
  • 【文献出处】 中国中药杂志 ,China Journal of Chinese Materia Medica , 编辑部邮箱 ,2016年02期
  • 【分类号】R284.1;O657.63
  • 【被引频次】5
  • 【下载频次】393
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