HPLC-ESI-MS/MS同时测定松萝中3种酚酸类成分的含量  

Simultaneous determination of 3 phenolic acids in Usnea by HPLC-ESI-MS/MS

作　　者：马英华[1] 田婷婷[1] 解伟伟 靳怡然[2] 许慧君[1] 张兰桐[1] 杜英峰[1] 

机构地区：[1]河北医科大学药学院药物分析教研室,河北石家庄050017 [2]河北医科大学第二医院药学部,河北石家庄050000

出　　处：《中国中药杂志》2015年第24期4884-4889,共6页China Journal of Chinese Materia Medica

基　　金：国家自然科学基金项目(81402894)

摘　　要：建立高效液相色谱串联质谱法(HPLC-ESI-MS/MS)同时测定松萝中松萝酸、地弗地衣酸、拉马酸3种主要有效成分的含量。采用Agilent ZORBAX SB-C18色谱柱(4.6 mm×250 mm,5μm),流动相为甲醇(0.05%甲酸)-水(0.05%甲酸-4 mmol乙酸铵),等度洗脱,流速0.8 m L·min^(-1)。采用正负离子切换模式,多反应监测(MRM)进行定量测定,在负离子条件下测定松萝酸和地弗地衣酸,在正离子条件下测定拉马酸。结果上述3种主要成分在进样量范围内呈良好线性(r>0.997 9);平均回收率为95.0%~105.1%,RSD为1.1%~5.2%。该方法简便、快速、准确、重复性好,为综合评价松萝的质量提供参考。A quick HPLC-ESI-MS/MS method was established for simultaneous determination of three chemical compositions in Usnea, including usnic acid, diffractaic acid, and ramalic acid. The separation was performed on a chromatographic column of Agilenl ZORBAX SB-C18（4.6 mm×250 mm,5μm ） , and the mobile phase was methanol （0. 05% fornfic acid）-0. 05% formic acid solution （4 mmol ammonium acetate） , with an isocratic elution at a flow rate of 0. 8 ml · min-1. Multiple reaction monitoring scanning mode （MRM） was performed combined with the ion switching technology in positive and negative ion switching mode to apply tot the quanti- tative determination. The calibration curves for the above three compounds were linear in corresponding injection amount. Their average recoveries were 95.0% -105.1% , with RSDs of 1.1% -5.2%. The method was simple, rapid, accurate with high repeatability, which could provide a reference for overcalling evaluation the quality of Usnea.

关 键 词：松萝 液相色谱-串联质谱 松萝酸 地弗地衣酸 拉马酸 定量 

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