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首页> 外文期刊>Analytical and bioanalytical chemistry >Analyzing small samples with high efficiency: Capillary batch injection-capillary electrophoresis-mass spectrometry
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Analyzing small samples with high efficiency: Capillary batch injection-capillary electrophoresis-mass spectrometry

机译:高效分析小样品:毛细管批量进样-毛细管电泳-质谱法

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摘要

We present an experimental approach to conducting fast capillary electrophoresis-mass spectrometry (CE-MS) measurements of very small samples in the nanoliter range. This is achieved by injecting sample very efficiently into a CE-MS system. Injection efficiency represents the ratio of injected sample to the amount of sample needed for carrying out the injection process (v/v). In order to increase this injection efficiency from typical values of 10 ~(-3) to 10 ~(-7), the concept of capillary batch injection is used to build an automated, smallfootprint injection device for CE-MS. This device is capable of running true multi-sample measurement series, using minimal sample volumes and delivering an injection efficiency of up to 100 %. It is compatible with both aqueous and non-aqueous background electrolytes. As an additional benefit, CE-MS separations of a catecholamine model system in capillaries of 15 cm length under conditions of high electric field strength could be accomplished in 20 s with high separation efficiency. This report details design and specifications of the injection device and shows optimal parameter choices for injections with both high injection efficiency and high separation efficiency. Furthermore, a procedure is presented to coat the tip of a fused silica capillary with a silicone elastomer which acts as a seal between two capillaries.
机译:我们提出了一种实验方法,可以对纳升范围内的极小样品进行快速毛细管电泳质谱(CE-MS)测量。这是通过将样品非常有效地注入CE-MS系统来实现的。进样效率表示进样量与执行进样过程所需的样品量之比(v / v)。为了将这种注射效率从典型值10〜(-3)提高到10〜(-7),使用毛细管批量注射的概念来构建用于CE-MS的自动化,小尺寸注射装置。该设备能够运行真正的多样品测量系列,使用最少的样品量,并提供高达100%的进样效率。它与水性和非水性背景电解质兼容。另外一个好处是,在高电场强度条件下,在15 cm长的毛细管中,儿茶酚胺模型系统的CE-MS分离可以在20 s内完成,分离效率很高。该报告详细介绍了注射装置的设计和规格,并显示了具有高注射效率和高分离效率的最佳注射参数选择。此外,提出了用硅氧烷弹性体涂覆熔融二氧化硅毛细管的尖端的程序,该硅氧烷弹性体用作两个毛细管之间的密封。

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