首页> 外文期刊>Journal of mass spectrometry: JMS >Comprehensive characterization of Annonaceous acetogenins within a complex extract by HPLC-ESI-LTQ-Orbitrap? using post-column lithium infusion
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Comprehensive characterization of Annonaceous acetogenins within a complex extract by HPLC-ESI-LTQ-Orbitrap? using post-column lithium infusion

机译:HPLC-ESI-LTQ-Orbitrap对复杂提取物中的丙酮酸造血素进行全面表征?使用柱后锂输注

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摘要

Annonaceous acetogenins (AAGs) are a homogenous class of polyketides proposed as environmental neurotoxins. Previous dereplication studies of AAGs were limited by the use of low-resolution mass spectrometers. Only poor information in terms of structures was provided due to the limited fragmentation of protonated or sodium cationized species. An innovative approach, using reversed-phase high-performance liquid chromatography coupled to a hybrid linear ion trap / orbitrap mass spectrometer (LTQ-Orbitrap?), was therefore performed. Sensitivity was enhanced by post-column infusion of lithium, since AAGs have a high affinity for this cation. High level of structural information was obtained from low-energy-collision-induced dissociation fragmentation experiments of lithium-cationized AAGs ([M + Li]+ ions) as demonstrated with purified standards. The method was then applied to a total ethyl-acetate extract prepared from commercial soursop nectar (Annona muricata L.). The sensitivity, mass accuracy and specific fragmentation patterns proved to be particularly useful for characterization of the AAGs. Typical structural identification procedure and unexpected observations for specific structural types are illustrated, with major and minor compounds.
机译:丙酮酸单环生成素(AAGs)是一类同质的聚酮化合物,被认为是环境神经毒素。以前的AAG重复复制研究受到低分辨率质谱仪的限制。由于质子化或钠阳离子化物种的碎片化程度有限,仅提供了关于结构的不良信息。因此,执行了一种创新的方法,该方法使用了反相高效液相色谱与线性离子阱/轨道阱混合质谱仪(LTQ-Orbitrap?)结合使用。柱后注入锂可提高灵敏度,因为AAG对这种阳离子具有很高的亲和力。高水平的结构信息是从低能量碰撞诱导的锂阳离子化AAG([M + Li] +离子)的离解碎裂实验获得的,如纯化标准所示。然后将该方法应用于由商业刺五加花蜜(Annona muricata L.)制备的总乙酸乙酯提取物。灵敏度,质量准确性和特定的碎片模式证明对AAG的表征特别有用。说明了主要结构和次要化合物的典型结构鉴定程序和对特定结构类型的意外发现。

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