气相色谱-质谱法测定废液样品中化武相关化合物

Determination of chemical weapons convention-related compounds in waste samples by gas chromatography-mass spectrometry

国际禁化武组织(OPCW)每年定期对各缔约国实验室进行分析能力验证,确保指定实验室能够胜任真实样品分析任务。2021年第50次水平考试由OPCW中心实验室进行配样,共配制6个废液样品。采用气相色谱-质谱法对6个考试废液样品进行分析鉴定,最终检出7个化武相关化合物。通过液液萃取、改变色谱固定相选择性等方法,实现了目标物与背景干扰的有效分离;结合电子轰击电离、化学电离、串联质谱分析等方式,完成了目标化合物结构的准确鉴定,所得结果与考试后OPCW发布的添加化合物清单一致。在鉴定的化合物中有2个为新型化武相关化合物,对其进行了质谱碎裂分析,为相关化学战剂降解、洗消的后续研究提供参考。

Organization for the Prohibition of Chemical Weapons(OPCW) conducts the official proficiency tests annually among Member States' laboratories to ensure that the designated laboratories maintain the technical competence for the analysis of authentic samples.Six waste samples were prepared by the OPCW Laboratory for the 50th proficiency test in 2021.In this paper,all the six waste samples were analyzed by gas chromatographymass spectrometry,and seven compounds related to the Chemical Weapons Convention were detected.The target chemicals were effectively separated from the background substances by liquid-liquid extraction or column phase selectivity by different stationary phase selection.The structures of the seven compounds were unambiguously identified by the combination of electron ionization,chemical ionization and tandem mass spectrometry modes,and the results were consistent with the spiking chemical list released by OPCW after the test.Among the identified chemicals,there are two novel Chemical Weapon Convention-related chemicals.The fragmentation pathways were presented in details,which may provide useful reference for the subsequent investigation on degradation and decontamination of the related chemical warfare agents.