Talanta ( IF 5.6 ) Pub Date : 2017-05-13 , DOI: 10.1016/j.talanta.2017.05.024
Marc André Althoff , Andreas Bertsch , Manfred Metzulat , Thomas M. Klapötke , Konstantin L. Karaghiosoff
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The successful application of headspace (HS) and direct immersion (DI) solid phase microextraction (SPME) for the unambiguous identification and characterization of a series of toxic thiophosphate esters, such as Amiton (I), from aqueous phases and complex matrices (e.g. grass and foliage) has been demonstrated. A Thermo Scientific gas chromatograph (GC) – tandem mass spectrometer (MS/MS) system with a TriPlus RSH® autosampler and a SPME tool was used to investigate the effect of different parameters that influence the extraction efficiency: e.g. pH of the sample matrix and extraction temperature.
The developed methods were employed for the detection of several Amiton derivatives (Schedule II of the CWC) that are structurally closely related to each other; some of which are new and have not been reported in literature previously. In addition, a novel DI SPME method from complex matrices for the analysis of organophosphates related to the CWC was developed. The studies clearly show that DI SPME for complex matrices is superior to HS extraction and can potentially be applied to other related compounds controlled under the CWC.
中文翻译:

顶空和直接浸没固相微萃取在分析与化学武器公约有关的有机硫代磷酸盐中从水和复杂基质中的应用
顶空(HS)和直接浸入(DI)固相微萃取(SPME)的成功应用成功地从水相和复杂基质(例如草皮)中明确鉴定和表征了一系列有毒的硫代磷酸酯,例如Amiton(I)和树叶)已被证明。使用带有TriPlusRSH®自动进样器和SPME工具的Thermo Scientific气相色谱仪(GC)–串联质谱仪(MS / MS)系统来研究影响萃取效率的不同参数的影响:例如样品基质的pH和提取温度。
所开发的方法用于检测几种在结构上密切相关的Amiton衍生物(CWC附表II);其中一些是新的,以前没有文献报道过。此外,还开发了一种来自复杂基质的新型DI SPME方法,用于分析与CWC相关的有机磷酸盐。研究清楚地表明,用于复杂基质的DI SPME优于HS萃取,并有可能应用于CWC控制下的其他相关化合物。