OPCW第42次环境样品水平考试洗消废水中化武相关化合物的液相色谱-质谱分析
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摘要
采用液相色谱-质谱技术(LC-MS)对禁止化学武器组织(OPCW)第42次水平考试洗消废水中化武相关化合物进行了详细地分析。首先用高效液相色谱-四极杆飞行时间高分辨质谱(HPLC-Q-TOF MS)从3个洗消废水样品中分辨出空白、控制与模拟真实样品,在模拟真实样品中初步找到3种化武相关化合物;随后采用超高效液相色谱-三重四极杆质谱(UPLC-QQQ MS)对这3种化武相关化合物进一步分析,鉴定出模拟真实样品中的2-羟乙基乙烯基硫醚、二乙烯基砜和1,2-双-(2-羟乙基巯基)乙烷。并对流动相中添加的缓冲剂以及质谱电离碎裂电压与裂解途径进行了优化。所得结果与OPCW提供的配样清单完全一致。该方法可为芥子气洗消产物的分析研究提供参考。
A method of liquid chromatography-mass spectrometry( LC-MS) was used to analyze the chemical weapon related compounds in the aqueous decontamination effluent samples of the 42 ndOfficial Organization for the Prohibition Chemical Weapons( OPCW) Proficiency Test. Firstly,the blank sample,control sample and simulated sample were distinguished by HPLC-Q-TOF MS from the three aqueous decontamination effluent samples,then three chemical weapon related compounds were preliminarily found out in simulated sample. Finally,2-hydroxyethyl vinyl sulfide,divinyl sulfone and 1,2-bis( 2-hydroxyethylthio) ethane in the simulated sample were identified simultaneously by UPLC-QQQ MS. The buffer agents,fragmentor voltages and fragmentation pathway were discussed adequately. The results obtained were in accordance with the list of spiking chemicals provided by the laboratory of OPCW. The method could provide a reference for the analysis on the decontamination products of sulfur mustard.
A method of liquid chromatography-mass spectrometry( LC-MS) was used to analyze the chemical weapon related compounds in the aqueous decontamination effluent samples of the 42 ndOfficial Organization for the Prohibition Chemical Weapons( OPCW) Proficiency Test. Firstly,the blank sample,control sample and simulated sample were distinguished by HPLC-Q-TOF MS from the three aqueous decontamination effluent samples,then three chemical weapon related compounds were preliminarily found out in simulated sample. Finally,2-hydroxyethyl vinyl sulfide,divinyl sulfone and 1,2-bis( 2-hydroxyethylthio) ethane in the simulated sample were identified simultaneously by UPLC-QQQ MS. The buffer agents,fragmentor voltages and fragmentation pathway were discussed adequately. The results obtained were in accordance with the list of spiking chemicals provided by the laboratory of OPCW. The method could provide a reference for the analysis on the decontamination products of sulfur mustard.
引文
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[2] Dubey V,Velikeloth S,Sliwakowski M,Mallard G. Accredit. Qual. Assur.,2009,14(8):431-437.
[3] Praveen K J,Prasad G K,Ramacharyulu P V R K,Singh B,Anchal R S. J. Alloys Compd.,2017,692:833-840.
[4] Sheng H M,Williams P E,Tang W J,Riedeman J S,Zhang M L,Kenttmaa H I. J. Org. Chem.,2014,79(7):2883-2889.
[5] Hooijschuur E W J,Kientz C E,Hulst A G,Brinkman U A T. Anal. Chem.,2000,72(6):1199-1206.
[6] Tang W J,Sheng H M,Kong J Y,Yerabolu R,Zhu H Y,Max J,Zhang M L,Kenttmaa H I. Rapid Commun. Mass Spectrom.,2016,30(12):1435-1441.
[7] Singh R,Gutch P K,Mazumder A. Ind. Eng. Chem. Res.,2013,52(13):4689-4694.
[8] Hou Z H,Sun J H,Zheng W,Han S,Liu H Y,Ying Y,Sun P P,Zhang C,Wang H S,Zhao B Q. Disaster Med. Rescue:Electron. Ed.(侯志宏,孙景海,郑伟,韩松,刘红岩,应莺,孙培培,张城,王好山,赵宝全.灾害医学与救援:电子版),2014,3(2):74-78.
[9] Sirjean B,Lizardo-Huerta J C,Verdier L,Fournet R,Glaude P A. Proceedings of the Combustion Institute,2017,36(1):499-506.
[10] Li Z P,Chen Z S,Zhang L B. J. Instrum. Anal.(李增沛,陈志升,张兰波.分析测试学报),2007,(6):901-903.
[11] Yu H L,Chen Z S,Liu J Q,Yuan L,Zhang L B. J. Chin. Mass Spectrom. Soc.(于惠兰,陈志升,刘景全,袁铃,张兰波.质谱学报),2005,(4):211-214.
[12] Zhang L B,Zhang C H,Yu H L,Li X H,Liu J Q. Anal. Instrum.(张兰波,张春红,于惠兰,李欣海,刘景全.分析仪器),2014,(3):66-69.
[13] Mahato T H,Singh B,Srivastava A K,Prasad G K,Srivastava A R,Ganesan K,Vijayaraghavan R. J. Hazard Mater.,2011,192(3):1890-1895.
[14] McLafferty F W. Interpretation of Mass Spectra. 3rd ed. Wang G H,Jiang L F,Wang C H,transl. Beijing:Chemical Industry Press(麦克拉弗蒂F W.质谱解析. 3版.王光辉,姜龙飞,汪聪慧,译.北京:化学工业出版社),1999.
[15] Snyder R,Kirkland J,Glajch L. Pratical HPLC Method Development. Hoboken:John Wiley&Sons,2012:232-237.