摘要
目的:建立高效液相色谱-串联质谱法(LC-MS/MS)测定大鼠血浆中氧化白藜芦醇的浓度。方法:血浆样品经醋酸乙酯液液萃取处理。采用Venusil HILIC色谱柱(2.1 mm×150 mm,5.0μm)为分析柱,HILIC柱(4 mm×3.0mm,10.0μm)为保护柱,以乙腈-水(80∶20,其中含1 mmol·L-1甲酸铵)为流动相,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。用于定量氧化白藜芦醇和内标的MRM扫描离子通道分别为m/z243.1→175.1、227.1→143.0。每个样品的分析时间为5 min。结果:氧化白藜芦醇和内标的保留时间分别为1.95 min和1.80min。血浆中内源性物质对测定无干扰,氧化白藜芦醇的线性范围0.5～100 ng·mL-1,日内、日间精密度(RSD)均小于15%;检测血浆低、中、高3个浓度(1,10,80 ng·mL-1)氧化白藜芦醇苷的准确度分别为105.22%,100.50%,96.48%;检测血浆低、中、高3个浓度(1,10,80 ng·mL-1)氧化白藜芦醇的萃取回收率分别为70.54%,68.59%,73.24%。结论:本方法具有灵敏、准确、快速的特点,测定结果可靠,可用于氧化白藜芦醇苷的药动学研究。
OBJECTIVE To establish a liquid chromatography-tandem mass spectrometry （LC-MS/MS） method for the de- termination of oxyresveratrol in rat plasma. METHODS The plasma samples were extracted with acetoacetate. The extractive was separated on Venusil HILIC column （2. 1 mm× 150 ram, 5.0 μm） guarded by a HILIC column （4 minx 3.0 mm, 10. 0μm）. The mobile phase consisted of acetonitrile-water （80：20, containing i mmol. L-1 ammonium formate） at flow rate of 0, 3 mL.min-1. The injection volume was 10 μL and resveratrol was used as the internal standard （IS）. Eleetrospray ionization （ESI） source was applied and operated in the negative multiple reaction monitoring （MRM） mode. Oxyresveratrol and trans- resveratrol were detected on MRM by the transitions from the precursor to the product ion （m/z 243.1→175.1 and 227. 1→ 143.0）. And the total running time was 5 rain. RESULTS The retention time of oxyresveratrol and resveratrol was 1.95 rain and 1.80 min respectively. Chromatograms showed no endogenous interfering peaks with blank samples. The linear calibration curve was obtained over the concentration on range of 1-100 ng,mL-1. The limit of quantification was 1 ng. mL-1. The extrac- tion recovery ,has 70.54% ,68. 59% ,73.24% for low, middle and high QC samples. At the same time, the inter- and intra- day precision （RSD） was Iess than 15% and the average recovery were 105.22%, 100. 50% and 96. 48%. CONCLUSION The method is simple, sensitive and accuracy, and it is suitable for plasma concentration determination of oxyresveratrol.
出处
《中国医院药学杂志》
CAS
CSCD
北大核心
2013年第21期1783-1786,共4页
Chinese Journal of Hospital Pharmacy
基金
深圳市科技计划项目(编号:201203293)
