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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| Published in | 分析化学 Vol. 43; no. 10; pp. 1526 - 1530 |
|---|---|
| Main Author | |
| Format | Journal Article |
| Language | Chinese |
| 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 | |
| Online Access | Get full text |
| ISSN | 0253-3820 |
| DOI | 10.11895/j.issn.0253-3820.150015 |
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| Abstract | 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。 |
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| AbstractList | 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。 建立了微池加压溶剂提取(μ-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μ-PLE静态提取两次,每次5 min,再用100 μL甲醇冲洗一次,得到约500 μL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/μL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PM25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. |
| Author | 郝亮 吴大朋 关亚风 |
| AuthorAffiliation | 中国科学院大连化学物理研究所,大连116023 中国科学院大学,北京100039 |
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| Author_FL | HAO Liang WU Da-Peng GUAN Ya-Feng |
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| Author_xml | – sequence: 1 fullname: 郝亮 吴大朋 关亚风 |
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| DocumentTitleAlternate | Determination of Dicarboxylic Acids in Fine Atmospheric Particles by Micro-Pressurized Liquid Extraction Coupled with Gas Chromatography-Mass Spectrometry |
| DocumentTitle_FL | Determination of Dicarboxylic Acids in Fine Atmospheric Particles by Micro-Pressurized Liquid Extraction Coupled with Gas Chromatography-Mass Spectrometry |
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| Keywords | 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 |
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| Notes | 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 |
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| PublicationYear | 2015 |
| Publisher | 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 中国科学院大连化学物理研究所,大连116023 |
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| Snippet | 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... 建立了微池加压溶剂提取(μ-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μ-PLE静态提取两次,每次5 min,再用100 μL甲醇冲洗一次,得到约500 μL提取液;氮气吹干后,60℃硅烷化衍生30... |
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| SubjectTerms | PM2.5 二元酸 大气细粒子 微池加压溶剂提取 水溶性有机物 |
| Title | 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 |
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