微池加压溶剂提取-气相色谱-质谱法定量测定大气细粒子中的二元酸  

Determination of Dicarboxylic Acids in Fine Atmospheric Particles by Micro-Pressurized Liquid Extraction Coupled with Gas Chromatography-Mass Spectrometry

作　　者：郝亮[1,2] 吴大朋[1] 关亚风[1] 

机构地区：[1]中国科学院大连化学物理研究所,大连116023 [2]中国科学院大学,北京100039

出　　处：《分析化学》2015年第10期1526-1530,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(Nos.21275144;21321064)资助~~

摘　　要：建立了微池加压溶剂提取（＂-PLE）-气相色谱-质谱测定大气细粒子中4种二元酸（丙二酸、丁二酸、戊二酸、己二酸）的分析方法。采用滤膜采集PM2.5样品,甲醇为溶剂,在80℃、8 MPa压力下＂-PLE静态提取两次,每次5 min,再用100＂L甲醇冲洗一次,得到约500＂L提取液;氮气吹干后,60℃硅烷化衍生30 min,衍生物加内标后,直接采用GC-MS进行定量分析。本方法测定加标滤膜中的4种常见二元酸,在0.2~20 ng/＂L进样浓度范围具有良好的线性,方法定量限为（按S/N=10计）0.15~0.47 ng/m3,回收率为92%~122%,相对标准偏差2.6%~11.8%。对大连星海湾大气PM2.5样品中丙二酸、丁二酸、戊二酸、己二酸的定量检出结果分别为64.6、50.0、41.8和20.2 ng/m3。The method of micro-pressurized liquid extraction（ μ-PLE） coupled with gas chromatography-mass spectrometry for the analysis of 4 dicarboxylic acids（ DCAs,including malonic acid,succinic acid,glutaric acid,and adipic acid） in fine atmospheric particles was developed. PM2. 5filter sample was extracted byμ-PLE at a pressure of 8 MPa and temperature of 80℃ using methanol as extraction solution. After two static5-min extractions and a rinsing step with 100 μL of methanol,about 500 μL of extraction solution was obtained. The extraction solution was then blown to dry with high purity nitrogen and submitted to a silylation reaction for 30 min at 60℃. After internal standard（ IS） was added,derivatization solution was directly injected for GC-MS analysis. For quantification of 4 normally DCAs in fine atmospheric particles, the calibration curve was obtained with a good linear relationship in the range of 0. 2- 20 ng / μL. The limits of quantification（ LOQs,S / N = 10） were in the range of 0. 15- 0. 47 ng / m3. The recoveries were between 92%and 122% with the RSDs between 2. 6% and 11. 8% for spiked filter samples. The method was used to determine malonic acid,succinic acid,glutaric acid,and adipic acid in real PM2. 5samples collected from Xinghai Bay of Dalian city,and the results were determined to be 64. 6,50. 0,41. 8 and 20. 2 ng / m3 respectively.

关 键 词：大气细粒子 PM2.5 水溶性有机物 二元酸 微池加压溶剂提取 

分 类 号：X831[环境科学与工程—环境工程] O657.63[理学—分析化学]