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[摘要]
目的 建立扶正平消胶囊中苦杏仁苷、芍药苷、贝母素甲、黄芪甲苷和吴茱萸次碱5种成分的HPLC-MS测定方法。方法 色谱条件:色谱柱为Agilent Eclipse plus C18柱(250 mm×4.6 mm,5 μm),乙腈-0.1%甲酸水为流动相,梯度洗脱;质谱条件:采用电喷雾离子源(ESI),正离子检测,SIM模式。结果 苦杏仁苷、芍药苷、贝母素甲、黄芪甲苷和吴茱萸次碱的定量限分别为12.9、32.2、1.00、1.21、0.40 ng/mL,检测限分别为6.46、6.44、0.25、0.61、0.16 ng/mL;在相应的线性范围内r>0.999 0;峰面积之比的日内精密度(RSD)和日间精密度(RSD)均小于2%,平均回收率均在98%~102%。结论 本方法可同时测定扶正平消胶囊中苦杏仁苷、芍药苷、贝母素甲、黄芪甲苷和吴茱萸次碱的量,快速简便,实用性强。
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[Abstract]
Objective To simultaneously determine the contents of five components (amygdalin, paeoniflorin, peimine, astragaloside IV and rutaecarpine) in Fuzheng Pingxiao Capsula by LC-MS. Methods Chromatographic separation was achieved with gradient elution by Agilent Eclipse plus C18 column (250 mm × 4.6 mm, 5 μm) and an Agilent 1100 Mass Spectrometer system was operated under the SIM mode with electrospray positive ionization (ESI). The mobile phase is acetonitrile-0.1% methanoic acid. Results The LOQ of amygdalin, paeoniflorin, peimine, astragaloside IV, and rutaecarpine in Fuzheng Pingxiao Capsula were 12.9, 32.2, 1.00, 1.21, and 0.40 ng/mL, and the LOD were 6.46, 6.44, 0.25, 0.61, and 0.16 ng/mL, respectively. Within the linear range, r > 0.999 0. Both intra-day and inter-day precision with RSD was less than 2%. The average recovery rates of the five components were in the range of 98%—102%. Conclusion This method is fast, sensitive, and reproducible. It could be used to determine amygdalin, paeoniflorin, peimine, astragaloside IV, and rutaecarpine in Fuzheng Pingxiao Capsula under the same chromatogram condition.
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