色谱

色谱

• 研究论文 • 上一篇    下一篇

气相色谱-串联质谱法测定土壤中的邻苯二甲酸酯

李红*, 田福林, 任雪冬, 王歆睿   

  1. 辽宁省分析科学研究院 辽宁省标准化体系建设工程技术研究中心, 辽宁 沈阳 110015
  • 收稿日期:2011-01-17 修回日期:2011-03-14 出版日期:2011-06-28 发布日期:2011-07-25
  • 通讯作者: 李红,硕士. Tel: (024)24211241
  • 基金资助:

    辽宁省博士科研启动基金项目(No. 20101051)

Determination of phthalic acid esters in soil by gas chromatography-tandem mass spectrometry

LI Hong*, TIAN Fulin, REN Xuedong, WANG Xinrui   

  1. Liaoning Province Academy of Analytic Sciences, Standard System Engineering Research Center of Liaoning Province, Shenyang 110015, China
  • Received:2011-01-17 Revised:2011-03-14 Online:2011-06-28 Published:2011-07-25

PDF

655

被引次数

56

摘要： 建立了土壤中6种邻苯二甲酸酯的气相色谱-串联质谱(GC-MS/MS)分析方法。土壤样品用超声提取,以二氯甲烷-丙酮(1:1, v/v)混合溶液为提取溶剂,提取液经Florisil小柱净化后,经HP-5MS色谱柱(30 m×0.25 mm×0.25 μm)分离,利用MS/MS的多反应监测(MRM)模式进行定性和定量。结果表明本方法可对样品中的邻苯二甲酸酯进行分析,在10～1000 μg/L质量浓度范围内,线性关系良好,相关系数为0.9973～0.9976;6种邻苯二甲酸酯的相对标准偏差(RSD)不大于14.3%, 2 μg/kg和10 μg/kg两个加标水平的回收率为72.9%～106.2%; 6种目标化合物的检出限为0.1～0.5 μg/kg。该方法快速准确、背景干扰较少、分析灵敏度较高,适用于土壤样品中邻苯二甲酸酯的分析。

关键词: 串联质谱, 邻苯二甲酸酯, 气相色谱, 土壤, 增塑剂

Abstract: A method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the determination of phthalic acid esters (PAEs) in soil. The soil sample was extracted by dichloromethane-acetone (1:1, v/v) with an ultrasonic instrument, and the extract was cleaned up with a Florisil column. The identification and quantification of the analytes were carried out in the multiple reaction monitoring (MRM) mode after the GC separation on an HP-5MS column (30 m×0.25 mm×0.25 μm). The eight point calibration curves showed a good linearity for all the congeners (0.9973~0.9976). The limits of detection (LODs) ranged from 0.1 to 0.5 μg/kg. The relative standard deviations(RSDs) were not more than 14.3% and the spiked recoveries were in the range of 72.9%~106.2%. The developed analytical method is rapid and accurate, and suitable for the determination of PAEs in soil.

Key words: soil, gas chromatography (GC), phthalic acid esters (PAEs), plasticizer, tandem mass spectrometry (MS/MS)