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Pilot for Validation of Online Pretreatments for Analyses of Organics by Gas Chromatography-Mass Spectrometry: Application to Space Research

机译:气相色谱-质谱联用分析有机物在线预处理方法的试验:在空间研究中的应用

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The search for complex organic molecules in extraterrestrial environments, including important biomolecules such as amino and fatty adds, will require a space compatible sample handling system to enable their detection by gas chromatography-mass spectrometry (GC-MS). For the future Mars exploratory mission Exomars 2018 aimed at organic molecules detection, a dedicated laboratory pilot, called Device for Pretreatment of Sample (DPS), reproducing representative space operating conditions has been developed. After its optimization, it aimed at validating under development protocols and interpreting forthcoming in situ resulting data. The DPS, dedicated to organic compounds' analysis, is discussed in terms of its technical features. The derivatization is carried out on a 50-100 mg mineral sample in a 4 mL reactor coupled with a GC-MS injector to simulate on line in situ derivatization-volatilization-transfer steps. Three derivatization reactions have been carried out with N-methyl-N-(tent-butyldimethylsilyL)-trifluoroacetamide (MTBSTFA) as silylating reagent, N,N-dimethylformamide dimethylacetal (DMF-DMA) and tetramethylammonium hydroxide (TMAH) as methylating agents. The performances are illustrated by comparison of conventional and in situ silylation, developed for space research applications, using terrestrial mineral matrix and Mars analog materials enriched with 25 nmol of each targeted organic molecule. The work presented in this rationale has established that the use of derivatization reactions widens the scope of targeted molecules but also clearly points out mineral matrix effect. Decreasing mineral influence on pretreatment will be the next scientific challenge in in situ analysis.
机译:在地外环境中寻找复杂的有机分子,包括重要的生物分子,例如氨基和脂肪添加物,将需要空间兼容的样品处理系统,以使其能够通过气相色谱-质谱(GC-MS)进行检测。对于旨在针对有机分子检测的未来火星探索任务Exomars 2018,开发了一种专门的实验室飞行员,称为样品预处理装置(DPS),可再现代表性的太空运行条件。经过优化后,它旨在验证开发协议并解释即将到来的结果数据。专门针对有机化合物分析的DPS的技术特点进行了讨论。衍生化是在4 mL反应器中,将50-100 mg矿物样品与GC-MS进样器耦合进行的,以在线模拟原位衍生化-挥发-转移步骤。已使用N-甲基-N-(帐篷丁基二甲基甲硅烷基)-三氟乙酰胺(MTBSTFA)作为甲硅烷基化试剂,N,N-二甲基甲酰胺二甲基乙缩醛(DMF-DMA)和四甲基氢氧化铵(TMAH)作为甲基化试剂进行了三个衍生化反应。通过比较传统的和原位的甲硅烷基化来说明这些性能,这些硅烷化是为空间研究应用开发的,使用的是陆地矿物基质和富含25 nmol每个目标有机分子的火星类似物。该基本原理提出的工作已经确定,衍生化反应的使用扩大了目标分子的范围,但也明确指出了矿物基质效应。减少矿物对预处理的影响将是原位分析中的下一个科学挑战。

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