UPLC-MS/MS同时测定桂枝茯苓胶囊中6种三萜酸类成分的含量

Simultaneous determination of six triterpenoid acids from Guizhi Fuling capsules by UPLC-MS/MS

建立超高效液相色谱-质谱联用(UPLC-MS/MS)同时测定桂枝茯苓胶囊中6种三萜酸类成分含量的分析方法。采用Agilent Porosheell 120 SB-C_(18)柱(4.6 mm×150 mm,2.7μm);流动相为0.1%甲酸水溶液-甲醇,梯度洗脱,流速0.4 m L·min^(-1),柱温30℃;进样量5μL。质谱条件采用电喷雾离子(ESI)源,多重反应监测(MRM)扫描,定量离子对为m/z 527.8→465.5(茯苓酸),m/z 525.6→465.6(去氢茯苓酸),m/z 483.4→337.3(去氢土莫酸),m/z 481.5→419.5(猪苓酸C),m/z467.4→337.1(去氢齿孔酸),m/z 453.4→337.0(松苓新酸)。结果显示,6种三萜酸类成分在进样质量浓度范围内呈现良好的线性关系(r>0.996 8),精密度RSD<6.2%;重复性RSD<5.9%,平均回收率分别为97.90%,100.2%,99.60%,101.7%,102.6%,103.0%。该方法准确、快速、重复性好,实现了中药成方制剂中茯苓三萜酸类成分的定量测定,可为桂枝茯苓胶囊的质量控制提供参考方法;并为含茯苓的中药成方制剂中建立含量测定方法提供参考。

To establish a UPLC-MS/MS method for simultaneous determination of six triterpenoid constituents（ pachymic acid,dehydropachymic acid,dehydrotumulosic acid,polyporenic acid C,dehydroeburicoic acid and dehydrotra metenolic acid） in Guizhi Fuling capsules（ GFC）. Chromatographic analysis was conducted on Agilent Porosheell 120 SB-C_（18）column（ 4. 6 mm × 150 mm,2. 7μm）,with 0. 1% formic acid aqueous solution-methanol as the mobile phase for gradient elution at a flow rate of 0. 4 m L·min^（-1）. The column temperature was 30 ℃ and the sample size was 5 μL. The samples were analyzed by tandem mass spectrometer with negative electrospray ionization（ ESI） source,and monitored under a multiple reaction monitoring（ MRM） mode,with the quantitative ion pairs m/z 527. 8 →465. 5（ pachymic acid）,m/z 525. 6 →465. 6（ dehydropachymic acid）,m/z 483. 4 →337. 3（ dehydrotumulosic acid）,m/z 481. 5→419. 5（ polyporenic acid C）,m/z 467. 4→337. 1（ dehydroeburicoic acid）,m/z 453. 4→337. 0（ dehydrotra metenolic acid）. Six triterpenoid acids showed good linear relationships within the investigated concentration ranges（ r 0. 996 8）,with RSDs of precision less than 6. 2%,and all RSDs of repeatability less than 5. 9%. The average recovery rate was 97. 90%,100. 2%,99. 60%,101. 7%,102. 6% and 103. 0% respectively. The method was rapid,accurate,repeatable and could be used as a method for quantitative determination of triterpenoid acids in Chinese medicine prescriptions,providing a reference method for the quality control of Guizhi Fuling capsules and providing a reference for the content determination for Chinese medicine prescriptions containing Poria cocos.