Analyzing small samples with high efficiency: capillary batch injection–capillary electrophoresis–mass spectrometry
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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, small-footprint 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.
KeywordsInjection efficiency Fast capillary electrophoresis Hyphenation Mass spectrometry Small sample Fused silica capillaries High electric field strengths Catecholamines
Capillary batch injection
Time-of-flight mass spectrometry
We would like to thank the glass, mechanical, and electronic workshops at the University of Regensburg for their assistance in implementing the experimental setup. Financial support by the Deutsche Forschungsgemeinschaft (MA 1401/7-1) is gratefully acknowledged. This research was supported by the Research Executive Agency (REA) of the European Union under Grant Agreement number PITN-GA-2010-264772 (ITN CHEBANA).
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