• 主题
高级搜索  >
历史搜索 清空历史
首页> 外文期刊>The Journal of automatic chemistry >Headspace Solid-Phase Microextraction Coupled to Comprehensive Two-Dimensional Gas Chromatography Time-of-Flight Mass Spectrometry for the Determination of Short-Chain Chlorinated Paraffins in Water Samples
【24h】

Headspace Solid-Phase Microextraction Coupled to Comprehensive Two-Dimensional Gas Chromatography Time-of-Flight Mass Spectrometry for the Determination of Short-Chain Chlorinated Paraffins in Water Samples

机译：顶空固相微萃取与二维气相色谱-飞行时间质谱联用，用于测定水中的短链氯化石蜡

获取原文
           
页面导航
  • 摘要
  • 著录项
  • 相似文献
  • 相关主题

摘要

Short-chain chlorinated paraffins (SCCPs) are a new type of persistent organic pollutants. In this work, a simple and effective method involving headspace solid-phase microextraction (HS-SPME) and comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC?×?GC-TOF-MS) was developed and optimized for the determination of trace SCCPs in water samples. The key parameters related to extraction and separation efficiency were systematically optimized. The SCCP congener groups were best resolved using an Rxi-5Sil MS (30?m?×?0.25?mm?×?0.25?μm) column followed by an Rxi-17Sil MS (1.0?m?×?0.15?mm?×?0.15?μm) column; the optimum extraction conditions were achieved with a 100?μm polydimethylsiloxane SPME fiber, when a 10?mL water sample added with 3.6?g sodium chloride was incubated for 15?min at 90°C and then extracted during 60?min at 90°C and desorption at 260°C for 2?min. The proposed method showed good linearity in the concentration range of 0.2–20.0?μg/L with the determination coefficient greater than 0.995. The detection and quantification limits ranged from 0.06 to 0.13?μg/L and 0.18 to 0.40?μg/L, respectively, which are sufficient to meet the regulatory detection limits as set by most environmental regulations. The accuracy and precision of the method was also good, where the recoveries ranged from 82.5 to 95.4%, and intra- and interday precision was within 7.2% and 14.5%, respectively. The optimized method has been applied to the determination of SCCPs in ten freshwater samples of three different types.
机译：短链氯化石蜡（SCCP）是一种新型的持久性有机污染物。在这项工作中，开发了一种简单有效的方法，涉及顶空固相微萃取（HS-SPME）和全面的二维气相色谱飞行时间质谱（GC？×？GC-TOF-MS）测定水样中的痕量短链氯化石蜡。系统地优化了与提取分离效率有关的关键参数。使用Rxi-5Sil MS（30？m？×？0.25？mm？×？0.25？μm）色谱柱和Rxi-17Sil MS（1.0？m？×？0.15？mm？× （0.15μm）色谱柱;最佳提取条件是使用100 µm的聚二甲基硅氧烷SPME纤维实现的，将10 µmL的水样品中加入3.6 µg氯化钠在90°C下孵育15分钟，然后在90°C下60分钟提取。并在260℃下解吸2分钟。所提出的方法在浓度范围为0.2–20.0？μg/ L时表现出良好的线性，测定系数大于0.995。检出限和定量检出限分别为0.06至0.13μg/ L和0.18至0.40μg/ L，足以满足大多数环境法规设定的法定检出限。该方法的准确性和精密度也不错，回收率在82.5％至95.4％之间，日内和日间精度分别在7.2％和14.5％之内。该优化方法已用于测定三种不同类型的十个淡水样品中的短链氯化石蜡。

著录项

相似文献

  • 外文文献
  • 中文文献
  • 专利
获取原文

客服邮箱：kefu@zhangqiaokeyan.com

京公网安备：11010802029741号 ICP备案号：京ICP备15016152号-6 六维联合信息科技 (北京) 有限公司©版权所有

  • 客服微信

  • 服务号