傅立叶变换离子回旋共振质谱法测定生物样品中的溶血磷脂酰胆碱  

Simultaneous Determination of Lysophosphatidylcholines in Biological Samples by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

作　　者：何凯丽 杨运云[2] 徐舸[1] 向章敏 HE Kai-li;YANG Yun-yun;XU Gel;XIANG Zhang-min(Department of Chemical Engineering,School of Science,Shenyang University of Technology,Shenyang 110870,China;Guangdong Engineering and Technology Research Center for Ambient Mass Spectrometry,Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals,Guangdong Institute of Analysis,Guangzhou 510070,China)

机构地区：[1]沈阳工业大学理学院化工系,辽中沈阳110870 [2]广东省测试分析研究所,广东省化学危害应急检测技术重点实验室,广东省原位电离质谱分析工程技术研究中心,广东广州510070

出　　处：《分析测试学报》2019年第12期1438-1443,共6页Journal of Instrumental Analysis

基　　金：广东省科学院发展专项资金项目(2019GDASYL-0302004,2018GDASCX0808,2017GDASCX0104).

摘　　要：建立了一种快速、同时测定复杂生物样品中4种溶血磷脂酰胆碱(LPCs)的傅立叶变换离子回旋共振质谱(FTICR-MS)分析方法。生物样品以甲醇-氯仿(9∶1,体积比)超声萃取30 min,离心后取上清液过0.22μm滤膜,进行FTICR-MS分析。质谱分析采用250μL微量进样器直接进样,进样流速为120μL/h;电喷雾(ESI)正离子模式检测,扫描质荷比范围为m/z 50~1 000,采用外标法进行定量分析。结果表明,4种LPCs在0.5~100μg/L质量浓度范围内呈良好的线性关系,相关系数(r^2)均不小于0.993 0。4种LPCs的检出限为0.02~0.03μg/L,定量下限为0.07~0.1μg/L。在血液和大鼠肝脏样本中,3个加标水平下4种LPCs的平均回收率为70.8%~95.0%,相对标准偏差(RSD)为1.2%~9.8%。该方法简单快速,灵敏度高,准确性和重复性好,适用于复杂生物样品中LPCs的快速测定。A Fourier transform ion cyclotron resonance mass spectrometric(FTICR-MS) method was developed for the simultaneous and rapid determination of four lysophosphatidylcholine(LPCs) in complex biological samples.The biological sample was ultrasonically extracted with methanol-chloroform(9 ∶ 1,by volume) for 30 min,and filtered with a 0.22 μm filter membrane for analysis.FTICR-MS determination were performed in direct infusion injection mode,using a 250 μL microsampler at a flow rate of 120 μL/h.MS spectra were recorded in a mass-to-charge ratio(m/z) range of 50-1 000 under positive ion electrospray ionization(ESI) mode.Quantitative analysis was conducted by the external standard method.Results indicated that the four investigated LPCs showed good linearity in the concentration range of 0.5-100 μg/L,with correlation coefficients(r^2) not less than 0.993 0.The limits of detection and quantitation were in the ranges of 0.02-0.03 μg/L and 0.07-0.1 μg/L,respectively.The average recoveries of four LPCs from plasma and rat liver samples at three spiked levels ranged from 70.8% to 95.0%,with relative standard deviations(RSD) of 1.2%-9.8%.The developed method showed the advantages of simplicity,rapidness,sensitivity,accuracy and good repeatability,and was suitable for the rapid determination of LPCs in complex biological samples.

关 键 词：傅立叶变换离子回旋共振质谱仪(FTICR-MS) 溶血磷脂酰胆碱(LPCs) 生物样品 

分 类 号：O657.23[理学—分析化学] Q946.0[理学—化学]