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搅拌棒吸附萃取与热脱附-离子迁移谱法测定水样中的三硝基甲苯和1,3,5-三硝基-1,3,5-三嗪

Stir-bar sorptive extraction and thermal desorption-ion mobility spectrometry for the determination of trinitrotoluene and l,3,5-trinitro-l,3,5-triazine in water samples.

作者信息

Lokhnauth John K, Snow Nicholas H

机构信息

Department of Chemistry and Biochemistry, Seton Hall University, 400 South Orange Avenue, South Orange, NJ 07079, USA.

出版信息

J Chromatogr A. 2006 Feb 10;1105(1-2):33-8. doi: 10.1016/j.chroma.2005.09.045. Epub 2005 Oct 24.

Abstract

Stir-bar sorptive extraction (SBSE) is interfaced to ion mobility spectrometry (IMS) for the rapid detection of trace analytes, with the explosives, trinitrotoluene (TNT) and l,3,5-trinitro-l,3,5-triazine (RDX) shown as examples. SBSE retains its inherent advantages as a sensitive, straightforward, solventless, and inexpensive method. Additionally, the new SBSE-IMS technique exhibits excellent sensitivity, has onsite field analysis capabilities and provides the potential to detect and quantitate analytes that are difficult to accomplish using gas chromatography (GC) or high-performance liquid chromatography (HPLC). The SBSE-IMS technique is shown to be an effective method for the low-level detection of TNT and RDX from water with method standard deviation of 8.6% for TNT and 6.6% for RDX. The short desorption time of 60 s and analysis time of less than 20 ms along with limits of detection of 0.1 ng/mL for TNT and 1.5 ng/mL for RDX and render the method potentially useful for trace analysis. Desorption profiles showing the kinetics of analyte transfer from the stir-bar into the IMS are shown and discussed; the SBSE-IMS configuration shows very rapid desorption from the stir-bar, with the analytes completely transferred in most cases, in under 1 min.

摘要

搅拌棒吸附萃取(SBSE)与离子迁移谱(IMS)联用,用于快速检测痕量分析物,以炸药三硝基甲苯(TNT)和1,3,5-三硝基-1,3,5-三嗪(RDX)为例进行说明。SBSE作为一种灵敏、直接、无溶剂且廉价的方法,保留了其固有的优势。此外,新的SBSE-IMS技术具有出色的灵敏度,具备现场分析能力,并为检测和定量那些使用气相色谱(GC)或高效液相色谱(HPLC)难以完成的分析物提供了可能。结果表明,SBSE-IMS技术是一种从水中低水平检测TNT和RDX的有效方法,TNT的方法标准偏差为8.6%,RDX为6.6%。60秒的短解吸时间和不到20毫秒的分析时间,以及TNT的检测限为0.1 ng/mL、RDX为1.5 ng/mL,使得该方法对痕量分析具有潜在的实用性。展示并讨论了解吸曲线,其显示了分析物从搅拌棒转移到IMS中的动力学;SBSE-IMS配置显示从搅拌棒的解吸非常迅速,在大多数情况下,分析物在不到1分钟的时间内就完全转移。

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