摘要
建立了大气颗粒物中有机胺类物质的气相色谱-质谱(GC-MS)分析方法。样品用超纯水超声萃取,然后在碱性条件下,用苯磺酰氯(Benzenesulfonyl chloride,BSC)衍生化,衍生物用二氯甲烷萃取,最后用DB-5MS色谱柱分离测定,实现了13种有机胺(包括7种脂肪胺、2种杂环胺和4种芳香胺)的同时测定。本方法的仪器检出限(S/N=3)和定量限(S/N=10)分别为0.00008~0.017μg/m L和0.00026~0.0565μg/m L;标准曲线线性相关系数为0.9903~0.9996,相关性良好;相对标准偏差(RSD)均小于30%,除低浓度加标水平的甲胺和苯甲胺,其余样品基质加标平均回收率为54.4%~159.7%,大部分胺具有较高的精密度与准确度。将本方法应用于广州城区PM^(2.5)样品的检测,共检出有机胺9种,其中甲胺、二甲胺和二丁胺约占9种有机胺总和的90%,是PM2.5中主要胺类物质,而丙胺浓度最低,浓度小于1.0 ng/m^3。
A method was developed for determination of thirteen amines including seven aliphatic amines,twoheterocyclic amines and four aromatic amines in atmospheric particulate matter(PM)by gas chromatographymassspectrometry(GC-MS).Samples were ultrasonically extracted with ultra-pure water and derivatized withbenzenesulfonyl chloride(BSC)under alkaline conditions.The derivatives were extracted withdichloromethane and then detected by GC-MS using DB-5MS chromatographic column.The method detectionlim it(S/N=3)and quantitation lim it(S/N=10)were0.00008-0.017滋g^mL and0.00026-0.0565滋g^mL respectively,and the correlation coefficients were0.9903-0.9996,which indicated that thestandard curve had good linear correlation.In addition,the relative standard deviation was less than30%andthe average recovery was54.4%-159.7%except for methylamine and benzylamine at spiked level of1.0滋g/m L,showing high precision and accuracy.9kinds of amines were detected in the PM2.5samplescollected in Guangzhou city by this method,among which dimethylamine and butylamine accounted for90%ofthe total nine amines,which indicated that they were primary amines in PM2.5;while propylamine exhibitedthe lowest level in PM2.5with the concentration less than1.0ng/m3.
作者
刘凤娴
毕新慧
任照芳
张国华
王新明
彭平安
盛国英
LIU Feng-Xian;BI Xin-Hui;REN Zhao-Fang;ZHANG Guo-Hua;WANG Xin-Ming;PENG Ping-An;SHENG Guo-Ying(State Key Laboratory of Organic Geochemistry,Guangzhou Institute of Geochemistry,Chinese Academy of Sciences, Guangzhou 510640,China;University of Chinese Academy of Sciences, Beijing 100049,China)
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2017年第4期477-482,共6页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金重大研究计划培育项目(No.91544101)资助~~
关键词
大气颗粒物
有机胺
气相色谱-质谱
Atmospheric particulates
Amines
Gas chromatography-mass spectrometry
