Kimm Gregory L, Hook Gary L, Smith Philip A
Uniformed Services University of the Health Sciences, Department of Preventive Medicine and Biometrics, Bethesda, MD 20814, USA.
J Chromatogr A. 2002 Sep 20;971(1-2):185-91. doi: 10.1016/s0021-9673(02)00999-8.
A field expedient analytical method for detecting the chemical warfare agent (CWA) sulfur mustard as a soil contaminant was developed using solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS). Five commercially available SPME fibers were investigated to determine the optimal fiber, and extraction conditions. Polyacrylate and carbowax-divinylbenzene fiber coatings gave a statistically indistinguishable and best response compared to the other three types examined in a simple system studied without soil. The polyacrylate fiber coating was selected for study of a system in which sulfur mustard was spiked to an agricultural soil (Standard Reference Material 2709, San Joaquin type). With soil samples, the greatest sensitivity occurred by the addition of deionized water to spiked soil and extraction at ambient temperature for 20 min or longer. SPME sampling with GC-MS analyses afforded good reproducibility (relative standard deviation between 2 and 10%), and analyte concentrations as low as 237 ng/g were detected in soil (total ion chromatograms). As completed here, total time for sampling and analysis was just under 1 h, and use of organic solvents or special sample introduction equipment was avoided.
开发了一种现场应急分析方法，用于检测作为土壤污染物的化学战剂（CWA）硫芥，该方法采用固相微萃取（SPME）和气相色谱-质谱联用（GC-MS）技术。研究了五种市售的SPME纤维，以确定最佳纤维和萃取条件。在一个不包含土壤的简单系统中研究发现，与其他三种类型的纤维涂层相比，聚丙烯酸酯和碳蜡-二乙烯基苯纤维涂层的响应在统计学上无显著差异且最佳。选择聚丙烯酸酯纤维涂层用于研究硫芥加标到农业土壤（标准参考物质2709，圣华金类型）中的系统。对于土壤样品，在加标土壤中加入去离子水并在室温下萃取20分钟或更长时间时，灵敏度最高。采用GC-MS分析的SPME采样具有良好的重现性（相对标准偏差在2%至10%之间），并且在土壤中检测到低至237 ng/g的分析物浓度（总离子色谱图）。按照此处完成的操作，采样和分析的总时间不到1小时，并且避免了使用有机溶剂或特殊的进样设备。
