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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
【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.
【Key words】 LC-MS/MS; Chuankezhi injection; 8-isoprenyl flavonoid glycoside; plasma concentration; quantitative analysis;
- 【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