Analytical Toxicology Branch, RDCB-DRT-T, US Army Edgewood Chemical Biological Center, Aberdeen Proving Ground, Maryland 21010-5424, USA.
Anal Chem. 2011 Feb 15;83(4):1315-20. doi: 10.1021/ac1024683. Epub 2011 Jan 14.
An analysis method has been developed for determining low parts-per-quadrillion by volume (ppqv) concentrations of nerve agent VX vapor actively sampled from ambient air. The method utilizes glass bead filled depot area air monitoring system (DAAMS) sampling tubes with isopropyl alcohol extraction and isotope dilution using liquid chromatography coupled with a triple-quadrupole mass spectrometer (LC/MS/MS) with positive ion electrospray ionization for quantitation. The dynamic range was from one-tenth of the worker population limit (WPL) to the short-term exposure limit (STEL) for a 24 L air sample taken over a 1 h period. The precision and accuracy of the method were evaluated using liquid-spiked tubes, and the collection characteristics of the DAAMS tubes were assessed by collecting trace level vapor generated in a 1000 L continuous flow chamber. The method described here has significant improvements over currently employed thermal desorption techniques that utilize a silver fluoride pad during sampling to convert VX to a higher volatility G-analogue for gas chromatographic analysis. The benefits of this method are the ability to directly analyze VX with improved selectivity and sensitivity, the injection of a fraction of the extract, quantitation using an isotopically labeled internal standard, and a short instrument cycle time.
已开发出一种分析方法,用于从环境空气中主动采样的痕量体积(ppqv)浓度的神经毒剂 VX 蒸气。该方法使用填充有玻璃珠的储库区域空气监测系统(DAAMS)采样管,用异丙醇提取,并用带有正离子电喷雾电离的液相色谱-串联质谱(LC/MS/MS)进行同位素稀释,以进行定量分析。动态范围从 1/10 工人职业接触限值(WPL)到 24 L 空气样品在 1 h 内的短时间接触限值(STEL)。使用液体加标管评估了该方法的精密度和准确性,并通过在 1000 L 连续流动室中收集痕量蒸气来评估 DAAMS 管的收集特性。与目前采用的热解吸技术相比,该方法具有显著的改进,后者在采样过程中利用氟化银垫将 VX 转化为用于气相色谱分析的更高挥发性 G 类似物。该方法的优点是能够直接分析 VX,具有更高的选择性和灵敏度,注入提取物的一部分,使用同位素标记的内标进行定量分析,以及仪器循环时间短。