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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 HPLC-ESI-MS / MS method was established for the simultaneous determination of the three main active constituents of Usneol, Diphenic Acid and Propimaric Acid in pineapple. The mobile phase consisted of methanol (0.05% formic acid) -water (0.05% formic acid-4 mmol ammonium acetate) using an Agilent ZORBAX SB-C18 column (4.6 mm × 250 mm, 5 μm) min ~ (-1). Positive and negative ion switching mode, multiple reaction monitoring (MRM) for quantitative determination of negative ions in the determination of liconic acid and diphenoxylate licorice, in the positive ion conditions for the determination of malic acid. Results The above three main components showed a good linearity (r> 0.997 9) within the range of injection volume. The average recoveries ranged from 95.0% to 105.1% with RSD ranging from 1.1% to 5.2%. The method is simple, rapid, accurate and reproducible, providing a reference for the comprehensive evaluation of the quality of Pinus.