摘要
建立了同时测定枳壳中川陈皮素和红橘素的UPLC-MS方法,并应用于大鼠血浆中的2种化学成分的浓度监测。色谱柱为Agilent Zorbax Eclipse Plus C_(18)柱(100 mm×2.1 mm,1.8μm);流动相为0.1%甲酸溶液-乙腈;体积流量0.6 m L/min;柱温30℃;进样量为5μL;采用电喷雾离子源正离子模式(ESI^+),多反应监测进行测定(MRM)。结果显示,川陈皮素和红橘素分别在1~500 ng/m L和1~750 ng/m L内具有良好的线性关系(r^2≥0.998),两成分的日内和日间精密度的RSD值均小于7.2%,准确度为95.2%~104.2%,基质效应在87.5%~114.6%合理范围内,平均回收率为85.5%~92.2%。本方法经方法学验证,可对川陈皮素和红橘素同时进行血药浓度检测,降低了分析成本,为临床用药研究提供了有效的分析手段。
An ultra-high performance liquid chromatographic method was established to simultaneously determine the contains of the nobiletin and tangeretin in Fructus aurantii （ZhiQiao）. This method was further applied in the determination of nobiletin and tangeretin in rat plasma after oral administration of ZhiQiao extract. The LC column was Agilent Zorbax Eclipse Plus C1s（100 mm^2.1 mm, 1.8 ~m）. The mobile phase was comprised of acetonitrile and water containing 0.1% formic acid. Flow rate was set at 0.6 mL/min. Column temperature was kept at 30~C. The quantification was obtained by scanning with multiple reaction monitoring （MRM） via the positive electrospray ionization （ESI~） source. The correlation coefficients of the nobiletin and tangeretin were respectively over 0.998 in the ranges of 1 ~500 ng/mL, 1 ~750 ng/mL. The RSD values of the inter-and intra-precisions were less than 7.2%. The accuracy ranged from 95.2% to 104.2%. The matrix effect values were sufficiently minimized to 87.5%-114.6%. The average recoveries from rat plasma were 85.5% to 92.2%. This method could significantly reduce the analysis cost, and provide an analytic method for the clinical medication adjustment.
出处
《精细化工中间体》
CAS
2017年第3期67-71,共5页
Fine Chemical Intermediates
基金
连云港市521人才资助项目(2016)
