正相固相萃取/GC-MS对强干扰有机样品中化学毒剂及相关化合物的测定

Analysis of Chemical Agents in Complex Organic Samples by GC-MS with Normal Solid-phase Extraction

建立了以硅胶键合氰基柱萃取、正己烷淋洗、混合溶剂分步洗脱,检测强干扰有机液体中化学毒剂及相关化合物的方法。沙林（GB）、梭曼（GD）、甲基膦酸二异丙酯（MPD IP）在0.50～50μg/L范围内,二甲胺基磷酸二乙酯（DEDMP）和维埃克斯（VX）在1.0～50μg/L范围内呈良好的线性关系;对强干扰有机样品中0.5和1.0 mg/L目标化合物的加标回收率均为34%～100%,且相对标准偏差均小于10%。所建立的方法,不仅消除了强干扰背景对气相色谱-质谱分析的影响,而且避免了目标化合物的丢失和降解,具有较高的实用价值。

A GC - MS method was developed for the determination of chemical agents, such as sarin （ GB ）, soman （ GD ）, diisopropyl methylphosphonate （ MPDIP）, diethyl dimethylphosphoramidate （DEDMP） and VX in complex organic samples by using normal solid-phase extraction. The chemical agents were extracted by the silica bonded cyanopropyl columella, washed by hexane and step-by-step eluted by mix solvents. Under the optimal conditions, the calibration curves showed good linearity in the range of 1.0 -50 μg/L for VX and DEDMP, and 0. 50 - 50μg/L for rest of compounds. The LODs of all target compounds were 0. 5 mg/L, and the recoveries of GB, GD, MPDIP, VX and DEDMP from organic sample spiked at two concentration levels of 0. 5 μg/L and 1.0 μg/L ranged from 34% - 100% with RSDs of less than 10%. The application of method for the determination of GB, GD, MPDIP, VX and DEDMP could not only eliminate the disturbance of a mass of diesel oil in organic samples, but also avoid the degradation and loss of the target compounds.