HILIC/LC-MS直接分离测定大气颗粒物中的15种有机胺  

Direct determination of fifteen amines in fine particles by HILIC/LC-MS

作　　者：刘智艺 王新锋 李敏 侯可勇 王一峰 LIU Zhiyi;WANG Xinfeng;LI Min;HOU Keyong;WANG Yifeng(Environment Research Institute,Shandong University,Qingdao 266237,China;School of Chemistry and Chemical Engineering,Shandong University,Jinan 250100,China)

机构地区：[1]山东大学环境研究院,青岛266237 [2]山东大学化学与化工学院,济南250100

出　　处：《地球环境学报》2023年第2期229-241,共13页Journal of Earth Environment

基　　金：山东省自然科学基金项目(ZR2020YQ30);国家重点研发计划(2020YFF01014503);山东大学基本科研业务费(2020QNQT012)。

摘　　要：本文建立了一种基于亲水作用液相色谱柱(HILIC)和液相色谱-质谱联用(LC-MS)的大气颗粒物有机胺的直接测定方法。颗粒物样品经甲醇提取、富集、浓缩后,对不同色谱柱与分析条件进行测试、对比,发现HILIC色谱柱可有效分离有机胺类化合物,高浓度以及低pH值的缓冲溶液可缩短大部分有机胺的保留时间,而流动相中有机相比例增加会延长保留时间。优化的HILIC/LC-MS分析方法可同时测定11种脂肪胺、2种脂环胺、1种芳香胺及1种醇胺,结合内标的有机胺标准曲线的线性相关系数R^(2)为0.991—0.999。本方法的检出限(S/N=3)为0.59—75.46 ng·mL^(-1),加标回收率为59%—92%,具有较高的精密度。该方法初步应用于青岛冬季大气细颗粒物样品中有机胺的测定,为大气有机胺的深入研究提供了方法参考与技术支撑。Background,aim,and scope Amines,ammonia derivatives with at least one hydrogen atom substituted by alkyl or aryl groups,are an important kind of nitrogen-containing organic compounds in the tropospheric atmosphere.Amines in fine particles constitute a significant fraction of secondary organic aerosols and have adverse effects on air quality and human health.However,due to the relatively high volatility,strong polarity,and low environmental concentration of low molecular weight amines,they are subjected to great difficulty in the accurate determination of their atmospheric abundances.So far amines have been measured in ambient aerosol particles by several techniques,including ion chromatography(IC),gas chromatography(GC),and high-performance liquid chromatography(HPLC).However,the determination with IC was limited to the low separation efficiency and resolution,while GC and HPLC were generally mandatory to use derivatization techniques to improve the separation efficiency and the detection limits.Due to derivatization processed could bring extra uncertainty on the determination of amines,in this study,a derivatization-free determination method based on LC-MS was developed to qualitatively and quantitatively measure particulate amines.Materials and methods The amine standards and the reagent chemicals in this study were ordered from Sigma-Aldrich(USA),AccuStandard(USA),Supelco(USA),TCI(Japan),and ALAF(USA).Particulate matters were collected on quartz fiber filters(Pall,USA)at a flow rate of 100 L·min^(−1) by a medium-volume fine particulate matter sampler from a rural site in coastal Qingdao.Samples were extracted with methanol,enriched and concentrated for qualitative and quantitative analysis.Amines in solutions were analyzed by using UHPLC(Ultimate 3000,Thermo Scientific,USA)coupled with a quadrupole mass spectrometer(MS,ISQ EC,Thermo Scientific)detector equipped with electrospray ionization(ESI)source.The separation of different amine compounds was performed with a hydrophilic interaction liquid chromatograp

关 键 词：有机胺 测定 HILIC 液相色谱-质谱联用仪 颗粒物 

分 类 号：X831[环境科学与工程—环境工程]