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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
【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。
【Abstract】 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 Agilent ZORBAX SB-C18( 4. 6 mm × 250 mm,5 μm),and the mobile phase was methanol( 0. 05% formic 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 for the quantitative 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.
【Key words】 Usnea; LC-MS/MS; usnic acid; diffractaic acid; ramalic acid; quantitation;
- 【文献出处】 中国中药杂志 ,China Journal of Chinese Materia Medica , 编辑部邮箱 ,2015年24期
- 【分类号】R284;O657.63
- 【被引频次】3
- 【下载频次】286