Kolakowski Beata M, D'Agostino Paul A, Chenier Claude, Mester Zoltán
NRC Institute for National Measurement Standards, 1200 Montreal Road, Ottawa, ON, Canada.
Anal Chem. 2007 Nov 1;79(21):8257-65. doi: 10.1021/ac070816j. Epub 2007 Sep 27.
Flow injection high field asymmetric waveform ion mobility spectrometry (FAIMS)-mass spectrometry (MS) methodology was developed for the detection and identification of chemical warfare (CW) agents in spiked food products. The CW agents, soman (GD), sarin (GB), tabun (GA), cyclohexyl sarin (GF), and four hydrolysis products, ethylphosphonic acid (EPA), methylphosphonic acid (MPA), pinacolyl methylphosphonic acid (Pin MPA), and isopropyl methylphosphonic acid (IMPA) were separated and detected by positive ion and negative ion atmospheric pressure ionization-FAIMS-MS. Under optimized conditions, the compensation voltages were 7.2 V for GD, 8.0 V for GA, 7.2 V for GF, 7.6 V for GB, 18.2 V for EPA, 25.9 V for MPA, -1.9 V for PinMPA, and +6.8 V for IMPA. Sample preparation was kept to a minimum, resulting in analysis times of 3 min or less per sample. The developed methodology was evaluated by spiking bottled water, canola oil, cornmeal, and honey samples at low microgram per gram (or microg/mL) levels with the CW agents or CW agent hydrolysis products. The detection limits observed for the CW agents in the spiked food samples ranged from 3 to 15 ng/mL in bottled water, 1-33 ng/mL in canola oil, 1-34 ng/g in cornmeal, and 13-18 ng/g in honey. Detection limits were much higher for the CW agent hydrolysis products, with only MPA being detected in spiked honey samples.
开发了流动注射高场不对称波形离子迁移谱(FAIMS)-质谱(MS)方法,用于检测和鉴定加标食品中的化学战(CW)剂。通过正离子和负离子大气压电离-FAIMS-MS对CW剂梭曼(GD)、沙林(GB)、塔崩(GA)、环己基沙林(GF)以及四种水解产物乙基膦酸(EPA)、甲基膦酸(MPA)、频哪基甲基膦酸(Pin MPA)和异丙基甲基膦酸(IMPA)进行分离和检测。在优化条件下,GD的补偿电压为7.2 V,GA为8.0 V,GF为7.2 V,GB为7.6 V,EPA为18.2 V,MPA为25.9 V,PinMPA为 -1.9 V,IMPA为 +6.8 V。样品制备尽量简化,每个样品的分析时间为3分钟或更短。通过在瓶装水、菜籽油、玉米粉和蜂蜜样品中加入低微克/克(或微克/毫升)水平的CW剂或CW剂水解产物,对所开发的方法进行了评估。在加标食品样品中观察到的CW剂检测限在瓶装水中为3至15 ng/mL,在菜籽油中为1至33 ng/mL,在玉米粉中为1至34 ng/g,在蜂蜜中为13至18 ng/g。CW剂水解产物的检测限要高得多,加标蜂蜜样品中仅检测到MPA。