LC-MS/MS分析血浆中脂肪酸及代谢产物  

Analysis of Fatty Acids and Metabolites in Plasma by LC-MS/MS

作　　者：钟宇 陈滨 李健 杨青锦 文娟 蔡春 ZHONG Yu , CHEN Bin, LI Jian, YANG Qing-jin , WEN Juan, CAI Chun(Analysis Center o f Guangdong Medical U niversity, Zhanjiang 524023, China)

机构地区：[1]广东医科大学分析中心,广东湛江524023

出　　处：《质谱学报》2018年第3期310-315,共6页Journal of Chinese Mass Spectrometry Society

基　　金：国家自然科学基金(21375029);湛江市科技攻关计划项目(2015B01025);广东医科大学科研基金(M2016021;XQ1303)资助

摘　　要：建立了高效液相色谱-串联质谱(LC-MS/MS)同时测定血浆中脂肪酸花生四烯酸(AA)及其代谢产物13-羟基十八碳烯酸(13-HODE)和9-羟基十八碳烯酸(9-HODE)的方法。采用Strata-X固相萃取柱净化,BEH C18色谱柱分离,以乙腈-水为流动相,流速0.2mL/min,等度洗脱;电喷雾离子源负离子模式和多反应监测模式定量。结果表明,3种物质在0.5~50μg/L范围内线性关系良好,相关系数为0.994 2~0.996 0;低、中、高3个加标水平的平均回收率为97.42%~101.46%;日内相对标准偏差为2.72%~6.11%,日间相对标准偏差为3.87%~6.39%;AA、13-HODE和9-HODE定量限分别为0.5、0.5、1.0μg/L。该方法简单、灵敏、快速、可靠,可用于血浆中脂肪酸及其代谢产物的检测分析。A method of liquid chromatography tandem mass spectrometry （LC-MS/MS）was developed for the determination of arachidonic acid （A A ） ,13-hydroxyoctadecadienoicacid （13-HODE） and 9-hydroxyoctadecadienoic acid （9-HODE） in plasma. The plasmasample was extracted using solid phase extraction, then separated on BEH C18 columnwith equal elution of acetonitrile and water as mobile phase, and the flow rate was0. 2 mL/min. It was detected by electrospray ionization tandem mass spectrometry inthe multiple reaction monitoring negative mode. The results show that A A , 13-HODEand 9-HODE have good linear relationship in the concentration of 0. 5-50 μg/L . Theaverage recoveries are 97. 42%-101. 46 % at 3 spiked levels. The precisions of intra-dayand inter-day are less than 6. 4% . The limits of quantification are 0. 5 ,0.5,1.0μg/L for AA , 13-HODE and 9-HODE, respectively. The method is simple, efficient and accurate, which is suitable for determination of fatty acids and metabolites in plasma.

关 键 词：血浆 3-羟基十八碳烯酸(13-HODE) 9-羟基十八碳烯酸(9-HODE) 花生四烯酸(AA) 液相色谱-串联质谱(LC-MS/MS) 

分 类 号：O657.63[理学—分析化学]