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搅拌棒吸附萃取-气相色谱-质谱联用测定海水中的邻苯二甲酸酯类物质

Detection of phthalate esters in seawater by stir bar sorptive extraction and gas chromatography-mass spectrometry.

作者信息

Si Qingqing, Li Fengmin, Gao Chenchen, Wang Cong, Wang Zhenyu, Zhao Jian

机构信息

College of Environmental Science and Engineering, Ministry of Education Key Laboratory of Marine Environment and Ecology, Qingdao Collaborative Innovation Center of Marine Science and Technology, Ocean University of China, Qingdao 266100, China.

Public Laboratory of Bioenergy and Biofuels, Qingdao Institute of Bioenergy and Bioprocess Technology, Chinese Academy of Sciences, No. 189 Songling Road, Qingdao 266101, China.

出版信息

Mar Pollut Bull. 2016 Jul 15;108(1-2):163-70. doi: 10.1016/j.marpolbul.2016.04.034. Epub 2016 May 2.

DOI:10.1016/j.marpolbul.2016.04.034
PMID:27157609
Abstract

We developed the stir bar sorptive extraction (SBSE)-gas chromatography-mass spectrometry (GC-MS) method to detect 15 kinds of PAEs in seawater. The stir bars (20mm in length and 1mm in film thickness) coated with 150μL of polydimethylsiloxane (PDMS) were found to demonstrate the optimal extraction of PAEs. The optimal conditions were as follows: extraction time of 2h, extraction temperature of 25°C, sodium chloride of 5%, methanol of 10%, analytical time of 50min, and methanol-acetonitrile (4:1) as the solvent. SBSE-GC-MS revealed that under the set temperature, the chromatographic peaks of all 15 PAEs can appear with complete separation. The detection limit ranged from 0.07μg/L to 5.71μg/L, whereas the limit of quantification ranged from 0.023μg/L to 193μg/L, and the correlation coefficients between the chromatographic peak area and concentration of the PAEs were greater than 0.92.

摘要

我们开发了搅拌棒吸附萃取(SBSE)-气相色谱-质谱联用(GC-MS)方法来检测海水中的15种邻苯二甲酸酯类物质。发现涂有150μL聚二甲基硅氧烷(PDMS)的搅拌棒(长度为20mm,膜厚为1mm)对邻苯二甲酸酯类物质具有最佳萃取效果。最佳条件如下:萃取时间2小时,萃取温度25°C,氯化钠浓度5%,甲醇浓度10%,分析时间50分钟,以及以甲醇-乙腈(4:1)作为溶剂。SBSE-GC-MS结果表明,在设定温度下,所有15种邻苯二甲酸酯类物质的色谱峰均可完全分离出现。检测限为0.07μg/L至5.71μg/L,定量限为0.023μg/L至193μg/L,邻苯二甲酸酯类物质的色谱峰面积与浓度之间的相关系数大于0.92。

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