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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。
A UPLC-MS method was developed for the simultaneous determination of nobiletrazine and tangerin in Fructus Aurantii and its application in the concentration monitoring of two chemistries in rat plasma. The column was Agilent Zorbax Eclipse Plus C 18 column (100 mm × 2.1 mm, 1.8 μm). The mobile phase consisted of 0.1% formic acid solution and acetonitrile. The volume flow rate was 0.6 m L / min. The column temperature was 30 ℃. 5μL; electrospray ionization positive ion mode (ESI ~ +), multiple reaction monitoring (MRM). The results showed that there was a good linear relationship between nobiletin and tangerine in the range of 1 ~ 500 ng / m L and 1 ~ 750 ng / m L (r ~ 2 ≥ 0.998). The intra- and inter-day precision RSD values were less than 7.2%, accuracy was 95.2% ~ 104.2%, matrix effect was within a reasonable range of 87.5% ~ 114.6%, the average recovery was 85.5% ~ 92.2%. This method is validated by methodology, which can be used for the simultaneous determination of nobiletin and tannin in blood serum, which reduces the cost of analysis and provides an effective means of analysis for clinical drug use.