UPLCMS/MS同时测定桂枝茯苓胶囊中6 种三萜酸类成分的含量(1)
[摘要] 建立超高效液相色谱质谱联用(UPLCMS/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 SBC18柱(4.6 mm×150 mm， 2.7 μm)；流动相为 0.1%甲酸水溶液甲醇，梯度洗脱，流速0.4 mL·min-1，柱温 30 ℃；进样量 5 μL。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/z 467.4→337.1(去氫齿孔酸)，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。
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[关键词] UPLCMS/MS； 桂枝茯苓胶囊； 三萜酸； 含量测定
Simultaneous determination of six triterpenoid acids from Guizhi Fuling
capsules by UPLCMS/MS
MA Ying1， LI Jiachun2， HUANG Wenzhe2， WANG Zhenzhong2， XIAO Wei2，SONG Yaling2， ZHANG Yongwen3*
(1. School of Chinese Pharmacy， Beijing University of Chinese Medicine， Beijing 100102， China；
2. Kanion Pharmaceutical Co.， Ltd.， Lianyungang 222001， China；
, 百拇医药
3. Center for Drug Evaluation， China Food and Drug Administration， Beijing 100038， China)
[Abstract] To establish a UPLCMS/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 SBC18 column (4.6 mm×150 mm， 2.7 μm)， with 0.1% formic acid aqueous solutionmethanol as the mobile phase for gradient elution at a flow rate of 0.4 mL·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., http://www.100md.com(马莹李家春 黄文哲 王振中 萧伟 宋亚玲 张永文)
, http://www.100md.com
[关键词] UPLCMS/MS； 桂枝茯苓胶囊； 三萜酸； 含量测定
Simultaneous determination of six triterpenoid acids from Guizhi Fuling
capsules by UPLCMS/MS
MA Ying1， LI Jiachun2， HUANG Wenzhe2， WANG Zhenzhong2， XIAO Wei2，SONG Yaling2， ZHANG Yongwen3*
(1. School of Chinese Pharmacy， Beijing University of Chinese Medicine， Beijing 100102， China；
2. Kanion Pharmaceutical Co.， Ltd.， Lianyungang 222001， China；
, 百拇医药
3. Center for Drug Evaluation， China Food and Drug Administration， Beijing 100038， China)
[Abstract] To establish a UPLCMS/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 SBC18 column (4.6 mm×150 mm， 2.7 μm)， with 0.1% formic acid aqueous solutionmethanol as the mobile phase for gradient elution at a flow rate of 0.4 mL·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., http://www.100md.com(马莹李家春 黄文哲 王振中 萧伟 宋亚玲 张永文)