高效液相色谱-串联质谱法测定大鼠血浆紫檀芪浓度  

Determination of Pterostilbene in Rat Plasma by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：郭润正[1] 吴春江[1] 张艳[1] 黄启慧[1] 李海峡[1] 王勖[1] 曹仲厚[1] 毛育华[2] 沈杰[2] 

机构地区：[1]交通部长江航务管理局疾病预防控制中心卫生检验所,武汉430019 [2]华中科技大学同济医学院公共卫生学院环境医学研究所教育部重点实验室,武汉430030

出　　处：《医药导报》2014年第1期27-30,共4页Herald of Medicine

基　　金：国家自然科学基金资助项目(21177046)

摘　　要：目的建立高效液相色谱一串联质谱法（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ThermoHy．psilGold色谱柱（2．1mm×50mm，5．0μm），保护柱为ThermoC18柱（4mm×3．0mm，10．0μm），以乙腈一水（含1mmol·L。甲酸铵）为流动相梯度洗脱，流速为0．3mL·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／z2 55．1—240．2，227．1—143．0。每个样品的分析时间为5min。结果紫檀芪和内标的保留时间分别为2．07，1．90min。血浆中内源性物质对测定无干扰，紫檀芪的线性范围为1—100ng·mL-1，日内、日间精密度（RSD）均〈15％；血浆低、中、高3种浓度（3，50，80ng·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（3，50，80ng·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 liquid chromatography-tandem mass spectrometry （LC-MS/MS） method for determination of pterostilbene in rat plasma. Methods The plasma samples were extracted with ethyl ether and then separated on Thermo Hypersil Gold column （2. 1 mm×50 mm, 5.0 μm）, and guarded by a Thermo C18 column （4 mm×3.0 mm, 10.0 μm）. The mobile phase consisted of acetonitrile-water （containing 1 mmol· L-1 ammonium formate） as gradient elution, and the flow rate was 0.3 mL·min-1. The injection volume was 10μL and resveratrol was used as the internal standard （IS）. Electrospray ionization （ESI） source was applied and operated in a negative mode using multiple reaction monitoring （MRM） . Pterostilbene and trans-resveratrol were detected on MRM by transition from the precursor to production （m/z 255.1-→240.2 and 227.1→143.0）. The total run time was 5 min. Results The retention time of pterostilbene and resveratrol was 2.07 and 1.90 min, respectively. No endogenous interfering peaks were observed. The linearity was obtained within the range of 1- 100 ng~ mL-l. The precision （RSD） of inter- and intra-day was less than 15% and the accuracy was 103.1% , 98.12% and 93.23% at low, mid, and high concentrations （3,50,80 ng ·mL-1） , respectively. The extraction recovery of pterostilbene was 78.6% , 80.3% and 83.2% , respectively, and no matrix effect was observed. Conclusion The method is simple, sensitive, accurate and reliable, which is suitable for pharmacokinetics study of pterostilbene.

关 键 词：紫檀芪 色谱-串联质谱法 高效液相 血浆浓度 

分 类 号：R282.71[医药卫生—中药学] R965[医药卫生—中医学]