加速溶剂萃取-高效液相色谱串联质谱法测定土壤中邻苯二甲酸酯  

Determination of 11 Phthalic Acid Esters in Soil by Accelerated Solvent Extraction-Liquid Chromatography Tandem Mass Spectrometry

作　　者：闫蕊[1,2] 邵明媛[1] 孙长华[2] 刘晓玲[2] 宋大千[1] 张寒琦[1] 于爱民[1] 

机构地区：[1]吉林大学化学学院,长春130012 [2]黑龙江省质量监督检测研究院,哈尔滨150050

出　　处：《分析化学》2014年第6期897-903,共7页Chinese Journal of Analytical Chemistry

基　　金：吉林省科技发展计划项目(No.20112102);教育部新世纪优秀人才项目(No.NECT-10-0443)

摘　　要：建立了高效液相色谱串联质谱技术（Liquid chromatography tandem mass spectrometry,LC-MS/MS）同时测定土壤中邻苯二甲酸酯（Phthalic acid esters,PAEs）的分析方法。确定了土壤样品加速溶剂萃取最优条件是以正己烷为萃取溶剂,在160℃下,静态萃取4次,每次12 min,萃取液经旋转蒸发浓缩,以乙腈-0.1%甲酸溶液为流动相梯度洗脱分离后,用LC-MS/MS结合大气压化学源（Atmospheric pressure chemical ionization,APCI）进行定性及定量分析。土壤中11种PAEs的浓度与其峰面积呈良好的线性关系,检出限为0.03-13.0μg/kg,样品的加标平均回收率为72.8%-101.8%,相对标准偏差（RSD）为1.7%-6.7%。方法简便快速,且灵敏度高,适用于土壤中11种邻苯二甲酸酯的同时测定。A sensitive and convenient method based on accelerated solvent extraction（ ASE）-liquid chromatography tandem mass spectrometry（ LC-MS / MS） was established for the simultaneous determination of 11 phthalic acid esters（ PAEs） in soil. The optimized conditions were as follows： By using n-hexane as the extraction solvent,spiked sample was extracted by ASE at 160 ℃ for 4 times,12 min for each time. The extract was concentrated by evaporation. Qualitative and quantitative analysis was carried out by the multiple reaction monitoring mode after the chromatographic separation with atmospheric pressure chemical ionization（APCI）,using acetonitrile -0. 1% formic acid water as mobile phase. The limits of detection（LODs） for 11 PAEs were between 0. 03- 13. 0 μg / kg. The recoveries and relative standard deviations were 72. 8%-101. 8% and 1. 7- 6. 7%,respectively. This method is rapid,sensitive and suitable for the determination of PAEs in soil.

关 键 词：加速溶剂萃取 高效液相色谱串联质谱法 大气压化学源 土壤 邻苯二甲酸酯 

分 类 号：X833[环境科学与工程—环境工程] O657.63[理学—分析化学]