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首页> 外文期刊>Journal of mass spectrometry: JMS >Identification and separation of saxitoxins using hydrophilic interaction liquid chromatography coupled to traveling wave ion mobility-mass spectrometry
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Identification and separation of saxitoxins using hydrophilic interaction liquid chromatography coupled to traveling wave ion mobility-mass spectrometry

机译：亲水相互作用液相色谱-行波离子淌度-质谱法鉴定和分离毒毒素

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摘要

The aim of this work was to develop a reliable and efficient analytical method to characterise and differentiate saxitoxin analogues (STX), including sulphated (gonyautoxins, GTX) and non-sulphated analogues. For this purpose, hydrophilic interaction liquid chromatography (HILIC) was used to separate sulphated analogues. We also resorted to ion mobility spectrometry to differentiate the STX analogues because this technique adds a new dimension of separation based on ion gas phase conformation. Positive and negative ionisation modes were used for gonyautoxins while positive ionisation mode was used for non-sulphated analogues. Subsequently, the coupling of these three complementary techniques, HILIC-IM-MS, permitted the separation and identification of STX analogues; isomer differentiation was achieved in HILIC dimension while non-sulphated analogues were separated in the IM-MS dimension. Additional structural characteristics concerning the conformation of STXs could be obtained using IM-MS measurements. Thus, the collision cross sections (CCS) of STXs are reported for the first time in the positive ionisation mode. These experimental CCSs correlated well with the calculated CCS values using the trajectory method. Copyright (c) 2015 John Wiley & Sons, Ltd.
机译：这项工作的目的是开发一种可靠而有效的分析方法，以表征和区分包括毒素（gonyautoxins，GTX）和未硫酸化类似物的毒素类毒素（STX）。为此目的，使用亲水相互作用液相色谱法（HILIC）分离硫酸化类似物。我们还采用离子迁移谱法来区分STX类似物，因为该技术增加了基于离子气相构象的分离新维度。淋菌毒素使用正电离和负电离模式，而未硫酸化的类似物则使用正电离模式。随后，这三种互补技术HILIC-IM-MS的结合使STX类似物得以分离和鉴定。在HILIC方面实现了异构体分化，而在IM-MS方面实现了无硫酸盐类似物的分离。使用IM-MS测量可以获得有关STX构象的其他结构特征。因此，在正电离模式下首次报告了STX的碰撞截面（CCS）。这些实验CCS与使用轨迹法计算的CCS值具有很好的相关性。版权所有（c）2015 John Wiley＆Sons，Ltd.

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