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目的建立高效液相色谱-串联质谱法(LC-MS/MS)测定大鼠血浆紫檀芪浓度。方法血浆样品经乙醚液液萃取处理。分析柱为Thermo Hypsil Gold色谱柱(2.1 mm×50 mm,5.0μm),保护柱为Thermo C18柱(4 mm×3.0 mm,10.0μm),以乙腈-水(含1 mmol·L-1甲酸铵)为流动相梯度洗脱,流速为0.3 mL·min-1,进样量10μL,内标为白藜芦醇,采用电喷雾离子源(ESI),以多反应监测(MRM)模式检测。用于定量紫檀芪和内标的MRM扫描离子通道分别为m/z 255.1→240.2,227.1→143.0。每个样品的分析时间为5 min。结果紫檀芪和内标的保留时间分别为2.07,1.90 min。血浆中内源性物质对测定无干扰,紫檀芪的线性范围为1~100 ng·mL-1,日内、日间精密度(RSD)均<15%;血浆低、中、高3种浓度(3,50,80 ng·mL-1)紫檀芪苷的准确度分别为103.10%,98.12%和93.23%;血浆低、中、高3种浓度(3,50,80 ng·mL-1)紫檀芪的萃取回收率分别为78.6%,80.3%和83.2%;检测方法不受基质效应影响。结论该方法灵敏、准确、快速,测定结果可靠,可用于紫檀芪的药动学研究。
Objective To establish a high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) for determination of plasma Pterostilbene in rats. Methods Plasma samples were extracted by ether liquid-liquid extraction. The analytical column was a Thermo Hypsil Gold column (2.1 mm × 50 mm, 5.0 μm) and the guard column was a Thermo C18 column (4 mm × 3.0 mm, 10.0 μm). The column was eluted with acetonitrile-water containing 1 mmol·L -1 ammonium formate ) Was used as mobile phase. The flow rate was 0.3 mL · min-1. The injection volume was 10 μL. The internal standard was resveratrol. Electrospray ionization (ESI) was used for the detection of multiple reaction monitoring (MRM) mode. The MRM scanning ion channels used for quantification of Pterostilbene and the internal standard were m / z 255.1 → 240.2, 227.1 → 143.0, respectively. The analysis time for each sample is 5 min. Results The retention time of Pterostilbene and internal standard was 2.07,1.90 min. The plasma endogenous substances had no interference with the determination. The linear range of Pteris strychni resveratrol was 1 ~ 100 ng · mL-1, the intra-day and inter-day precision (RSD) were less than 15%, and plasma low, middle and high concentrations 3,50,80 ng · mL-1). The accuracy of plasma was 103.10%, 98.12% and 93.23% respectively. The plasma concentrations of 3, 50, 80 ng · mL-1 The recoveries of stilbene were 78.6%, 80.3% and 83.2%, respectively. The detection method was not affected by the matrix effect. Conclusion The method is sensitive, accurate and rapid, and the determination results are reliable. It can be used to study the pharmacokinetics of.