采样管-固相微萃取法分析空气中的微量毒剂及相关化合物

Sampling Tube-Solid Phase Microextraction for Analyzing Toxicant and Relevant Compounds in Gas Samples

创立了采样管-SPME分析气体样品的新技术,并应用于对空气中微量毒剂及相关化合物的测定。对比了65μmPDMS/DVB纤维和50/30μmDVB/CAR/PDMS纤维对所选化合物的萃取效果。优化了萃取时间及解吸温度。通过对i-PrMPA的衍生方法研究,确定了在纤维涂层中衍生的方法。研究了采样管-SPME法测试DMMP、GB、i-PrMPA和GD的检出限,分别为56ng、84ng、121ng和274ng。

A new technique of sampling tube-solid phase microextraction （SPME） was developed. The target compound was collected in a sampling tube firstly, then the SPME fibre was placed over the adsorbent directly to extract the target compounds, finally the analytes were introduced into gas chromatograph by thermal desorption in the injection port. Heating the adsorbent in sampling tube is necessary for desorption of analytes. The capabilities of two commercial fibres [ （65μm, PDMS/ DVB） and （50/30μm, DVB/CAR/PDMS） ] were compared under different temperatures （from room temperature to 90℃）. Extraction time was l0 min. The result showed that the （65μm PDMS/DVB ） fibre is suitable for headspace extraction. With this fibre, the optimum extraction time was l0 min. Dervivatization in the fibre coating layer was also studied. The detection limits for dimethyl methylphosphonate, o-isopropyl ethylphosphonofluoridate, isopropyl methylphosphonate and pinacoly methylphosphonofluoridate were 56, 84, 121 and 274 ng, respectively.