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

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...

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Bibliographic Details
Published in分析化学 Vol. 43; no. 10; pp. 1526 - 1530
Main Author 郝亮 吴大朋 关亚风
Format Journal Article
LanguageChinese
Published 中国科学院大学,北京100039%中国科学院大连化学物理研究所,大连,116023 2015
中国科学院大连化学物理研究所,大连116023
Subjects
PM2.5
二元酸
大气细粒子
微池加压溶剂提取
水溶性有机物
二元酸
Fine atmospheric particle
水溶性有机物
微池加压溶剂提取
Dicarboxylic acids
PM2.5
大气细粒子
Micro-pressured liquid extraction
Water-soluble organic compounds
Online AccessGet full text
ISSN0253-3820
DOI10.11895/j.issn.0253-3820.150015

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Summary: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。
Bibliography:HAO Liang, WU Da-Peng, GUAN Ya-Feng（ Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China） （ University of Chinese Academy of Sciences, Beijing 100039, China）
22-1125/O6
Fine atmospheric particle; PM2.5; Water-soluble organic compounds; Dicarboxylic acids; Micro-pressured liquid extraction
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,derivatiza
ISSN:0253-3820
DOI:10.11895/j.issn.0253-3820.150015