第 47 卷第 3 期 Vol. 47 No. 3 2017 年 6 月 Jun 2017

所属栏目：分析与测试 UPLC-MS／MS法同时检测大鼠血浆中川陈皮素和红橘素的浓度

冯 里1，李天雪1，2*，胡玉涛1，2，韦 笑1 （1. 江苏联合职业技术学院 连云港中医药分院，江苏 连云港 222007；2. 连云港市药物研发共性技术中心，江苏 连云港 222007）

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 C18柱（100 mm×2.1 mm，1.8 μm）；流动相为0.1%甲酸溶液-乙腈；体积流量0.6 mL／min；柱温30℃；进样量为5 μL；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／mL和1～750 ng／mL内具有良好的线性关系（r2≥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。

关键词：枳壳；川陈皮素；红橘素；高效液相色谱质谱联用

中图分类号：　　文献标识码：A　　文章编号：1009-9212（2017）03-0067-05

Simultaneous Determination of the Nobiletin and Tangeretin in Rat Plasma by UPLC-MS/MS

FENG Li1, LI Tian-xue1,2*, HU Yu-tao1,2, WEI Xiao1 (1. Lianyungang TCM Branch of Jiangsu Union Technical Institute, Lianyungang 222007, China; 2. Lianyungang Common Technological Center for Drug Research and Development, Lianyungang 222007, China)

Abstract：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 C18(100 mm×2.1 mm, 1.8 μm). 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℃. 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．

Key words：Fructus aurantii L.; nobiletin; tangeretin; LC-MS/MS

基金项目：连云港市521人才资助项目（2016）。

作者简介：冯 里（1982-），男，江苏连云港人，硕士，讲师，主要从事药理学专业研究（E-mail：907773517@qq.com）。

联 系 人：李天雪，硕士，讲师，主要从事药物分析研究（E-mail：litx1988@126.com）。

收稿日期：2017-06-04