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LC-MS/MS法同时测定大鼠血浆中4种淫羊藿黄酮苷

Simultaneous determination of 4 prenylflavonoids of Chuankezhi injection in rat plasma by LC-MS/MS

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【作者】 许舜军朱雅玲余捷婧冯怡孙帅许艺镌杨柳

【Author】 XU Shun-jun;ZHU Ya-ling;YU Jie-jing;FENG Yi;SUN Shuai;XU Yi-juan;YANG Liu;Guangzhou Im Vin Pharmaceutical Co.Ltd.;Guangdong Second Traditional Chinese Medical Hospital;Guangdong Provincial Hospital of TCM, Guangdong Provincial Academy of Chinese Medical Sciences;

【机构】 广州万正药业有限公司广东省第二中医院广东省中医院广东省中医药科学院

【摘要】 建立大鼠血浆中朝藿定A、B、C及淫羊藿苷的LC-MS/MS法,并应用于大鼠肌肉注射喘可治注射液后血浆中4种黄酮苷浓度的测定及喘可治注射液的药物动力学研究。采用的色谱条件为Agilent Eclipse XDB-C18(150 mm×2.1 mm,5.0μm)色谱柱,乙腈-0.1%甲酸水溶液(35∶65)为流动相,流速0.22 mL·min-1,柱温40℃;质谱条件为电喷雾多反应离子监测(MRM)负离子检测模式,血浆样品采用固相萃取法处理。结果显示,朝藿定A、B、C及淫羊藿苷在11 000 ng·m L-1浓度内具有良好的线性关系;日内精密度RSD<5.99%,日间精密度RSD<10.16%;各成分相对回收率介于88.1%101.1%,RSD<7.9%,绝对回收率介于72.0%86.6%,RSD<6.3%。研究表明,该分析方法专属、灵敏、快速,适用于血浆中淫羊藿黄酮苷浓度的测定。

【Abstract】 A quantitative method for epimedin A, B, C and icariin in rat plasma was established using LC-MS/MS after intermuscular administration of Chuankezhi injection to rat. Chromatographic separation was performed on an Agilent Eclipse XDB-C18 column(150 mm × 2.1 mm, 5.0 μm) at 40 ℃. Mobile phase consisted of acetonitrile-0.1% formic acid in water(35∶65), and the flow rate was 0.22 m L·min-1. The LC effluent was detected and analyzed using an ESI-triple quadrupole tandem mass spectrometer under the multiple reaction monitoring(MRM) in the negative ion mode. The plasma samples were treated with solid phase extraction prior to LC-MS/MS analysis. As a result, all of the four analytes displayed a good linearity over the concentration of 1-1 000 ng·m L-1. The RSDs of intra-day and inter-day assays were less than 5.99% and 10.16%, respectively. The relative recovery of each analyte was between 88.1%-101.1% with RSD < 7.9% and the absolute recovery was between 72.0%-86.6%(RSD < 6.3%). In conclusion, the established method shows good specificity, sensitivity and efficiency for quantifying the four flavonoid glycosides contained in rat plasma.

  • 【文献出处】 药学学报 ,Acta Pharmaceutica Sinica , 编辑部邮箱 ,2016年04期
  • 【分类号】R285.5
  • 【被引频次】5
  • 【下载频次】397
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