摘要
目的 建立同时测定西洋参制剂中人参皂苷Rg1、Re、Rb1及抗疲劳类非法添加含量的液相色谱-质谱联用方法.方法采用Agilent ZORBAX SB-C18色谱柱（3.0mm×150mm,3.5μm）,流动相A为含0.1%乙酸的20mmol·L-1乙酸铵溶液,流动相B为甲醇∶乙腈（3：2）的混合溶液,采用线性梯度洗脱;流速为200μL·min-1,柱温35℃.质谱条件采用电喷雾离子化（ESI）方式,正负离子模式,以多级反应监控（MRM）模式对西地那非、伐地那非、他达拉非、人参皂苷Rg1、Re和Rb1进行含量测定.结果 西地那非、伐地那非、他达拉非、人参皂苷Rg1、Re和Rb1分别在2.99～59.85,0.43～8.60,3.32～66.42,3.16～63.29,2.63～52.68,4.15～82.93μg·mL-1浓度范围内与峰面积呈良好线性关系.西洋参制剂中西地那非、伐地那非、他达拉非、人参皂苷Rg1、Re和Rb1的平均加样回收率均介于92.9%～103.3%之间.结论 本法简单、快速、灵敏、准确,可用于西洋参制剂中西地那非、伐地那非、他达拉非、人参皂苷Rg1、人参皂苷Re和Rb1含量测定,为该药的质量控制提供依据.
OBJECTIVE To establish a LC-MS method for simultaneous determination of 6 compounds （Silde- nafil, Vardenafil, Tadalafil, Ginsenoside RgI , Re and Rb1 ） in American Ginseng Agent. METHODS The chromato- graphic separation was carried out at 35℃on a Aglient ZORBOX SB C18 column（3.0mm × 150mm,3.5μm） elated in a gradient program. Flow rate ：200μL . min-1. The mobile phase A consisted of water containing 20mmol . L-1 ammonium acetate and 0.1% Acetic acid. The mobile phase B was methanol-acetonitrile （3：2）. The mass spectra were obtained by Varian 310 triple quad mass spectrometer in MRM mode with eleetrospray ionization source in nega- tive and positive ion mode. RESULTS The linear ranges for Sildenafil, Vardenafil, Tadalafil. Ginsenoside Rg1,Re.and Rb1 were 2. 99 - 59.85,0. 43 - 8.60,3.32 - 66.42,3.16 -63.29,2. 63 - 52. 68,4. 15 - 82.93 μg . mL- 1, re- spectively. The average recoveries ranged between 92. 9% - 103.3%. CONCLUSION The established method is convenient,sensitive and accurate. It can be used for the determination of the contents of Sildenatil, Vardenafil, Tadalafil and Ginsenoside Rg1, Re and Rb1 in American Ginseng for quality control.
出处
《海峡药学》
2014年第2期47-50,共4页
Strait Pharmaceutical Journal
