摘要
为了准确测定小鼠血液中的Ⅳ一亚硝基降烟碱（NNN）及其代谢物，通过对色谱、质谱条件的优化，建立了以NNN—d4和HPB—d4为内标，用乙腈沉淀蛋白后，直接经超高效液相色谱（UPLC）仪器的亲水相互作用色谱（HILIC）柱进行分离，通过全扫描／数据依赖二级质谱扫描（FS／ddMS。）测定小鼠血浆中NNN及其7种代谢物的UPLC—QExactive轨道阱高分辨质谱法。结果表明：①NNN及其7种代谢物的检出限为0．019～0．067ng／mL，回收率在78．0％～117．5％之间，日内精密度为0．47％～8.38％。②该方法适合于小鼠血浆中NNN及其7种代谢物的同时检测。
In order to accurately determine the N-nitrosonornicotine （NNN） and its metabolites in mouse blood, a UPLC-Q Exactive orbit trap high-resolution mass spectrometry method was established by optimizing chromatographic and mass spectrometric conditions and using NNN-d4 and HPB-d4 as internal standards. Wherein, after protein precipitating with acetonitrile, the sample was separated directly by an HILIC column in UPLC spectrometer. NNN and its metabolites in mouse plasma were analyzed by mass spectrometry under full scan/data-dependent MS2 （FS/ddMS2） mode. The results showed that： 1） The limits of detection and the recoveries of NNN and its metabolites ranged from 0.019 to 0.067 ng/mL and from 78.0% to 117.5%, respectively, with the intra-day precision of 0.47%-8.38%. 2） The developed method was suitable for the simultaneous analysis of NNN and its seven metabolites in mouse plasma.
出处
《烟草科技》
EI
CAS
CSCD
北大核心
2015年第6期40-44,共5页
Tobacco Science & Technology
基金
国家自然科学基金面上项目"改性介孔材料固相萃取/UPLC-MSn方法研究烟草特有亚硝胺在动物体内的代谢"(21175153)
中国烟草总公司郑州烟草研究院院长科技发展基金项目"MIPs-SPE-HILIC-MSn在线分离鉴定平台的搭建及其在TSNAs分析中的应用"(602011CA0310)
