超高效液相三重四极杆质谱法快速检测生物体液中夹竹桃甙和甙元  

Rapid Determination of Oleandrin and Oleandrigenin in Biological Fluids by Ultra Performance Liquid Chromatography Triple Quadrupole Mass Spectrometry

作　　者：张秀尧[1] 蔡欣欣[1] 

机构地区：[1]温州市疾病预防控制中心,温州325001

出　　处：《分析化学》2011年第4期599-600,共2页Chinese Journal of Analytical Chemistry

基　　金：温州市医学重点学科项目;温州市第三轮"311"工程建设项目基金(No.2008012)资助

摘　　要：1引言 夹竹桃（Neriumoleander L.）是一种栽培常绿灌木,在温带、亚热带和热带地区广泛分布。夹竹桃全株含有强心甙类活性物质,有一定的药用价值,但也有相当的毒性。其主要有毒成分为夹竹桃甙（Oleandrin）及其甙元（Oleandrigenin）等,它们会抑制Na＋/K＋ATP酶活性,属迟效强心甙类,并有较强的致吐作用。Oleandrin and oleandrigenin,the major cardiac constituents of oleander（Nerium oleander L.）,were extracted from samples with tert-butyl methyl ether.The extract was dried under a stream of nitrogen gas,and the residue was dissolved in MeOH-H2O（1∶1,V/V）.The dissolved solution of plasma or vomit was defatted with-hexane and filtered through a microcentrifuge filter（3000 MW cut-off）.Chromatographic separation was performed on an UPLC BEH C18 column using gradient elution with 0.1% formic acid in 2 mmol/L ammonium acetate buffer-methanol,and detected by the positive electrospray ionization-MS/MS method under multiple reaction monitor mode.The cycle time of each analysis was 7.0 min.The average recoveries were 86.4%-116.0%,93.7%-111.0% and 92.3%-104.0% for oleandrin and oleandrigenin in plasma,urine and vomit,respectively,with RSDs of 3.4%-10.0%,2.3%-7.8% and 3.2%-7.2%（n=6）.The limits of quantitation（S/N=10） were 0.1 mg/L（mg/kg）.The method was simple,selective and sensitive to detect oleandrin and oleandrigenin for toxicological purposes.

关 键 词：夹竹桃 生物体液 快速检测 甙元 质谱法 四极杆 超高效 液相 

分 类 号：R284.1[医药卫生—中药学]