摘要
A method for the quantification of quercetin-3’-O-glucoside in rat plasma by high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was developed and validated.Along with internal standard(carbamazepine),quercetin-3’-O-glucoside was extracted from plasma samples by simple liquid-liquid extraction with ethyl acetate.The mass spectrometry detection was set in multiple reaction monitoring(MRM) mode via positive electrospray ionization(ESI).The chromatographic run time was 3.5 min per sample.The calibration curves were linear(r^2 = 0.9992) with a lower limit of quantification(LLOQ) of 10.625 ng/mL,and the limit of detection(LOD) was 4.25 ng/mL.The intra-and inter-day precision and accuracy,in terms of relative standard deviation(RSD),were all lower than 10.44%.The recovery rate of the analyte and internal standard were higher than 66.80%.After intravenous administration of 10 mg/kg quercetin-3’-O-glucoside,the t1/2 and AUC were(0.02±0.01) h and(1.22±0.28)×10^4 μg/L·h.The method is accurate,stable and sensitive,which is suitable for the pharmacokinetic study of quercetin-3’-O-glucoside in rats.
建立大鼠血浆中槲皮素-3'-O-葡萄糖苷的高效液相-串联质谱(HPLC-MS/MS)检测法。生物样品中槲皮素-3'-O-葡萄糖苷和卡马西平(内标)采用液-液萃取的方法提取,乙酸乙酯作为提取溶剂。HPLC-MS/MS方法采用多离子反应模式(MRM)进行检测,被测物质和内标均在3.5min内出峰。槲皮素-3'-O-葡萄糖苷在血浆中的最低定量限是10.625ng/mL,最低检测限是4.25ng/mL,平均回收率大于66.80%,日内、日间精密度和准确度的RSD值均小于10.44%。尾静脉注射10mg/kg槲皮素-3'-O-葡萄糖苷后,其t1/2和AUC分别是(0.02±0.01)h和(1.22±0.28)×104μg/L·h。本法准确、稳定、灵敏度高,适用于槲皮素-3'-O-葡萄糖苷的大鼠药代动力学研究。
基金
National Natural Science Foundation of China (Grant No. 30960494)
Jiangxi Province NSFC (Grant No. 2009 GZY0099)