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A combination of fast response liquid chromatography with nanospray mass spectrometry (FRL-MS) has been developed and applied to the analysis of amino acids, peptides, and proteins. After separation on a long monolithic (100 microm ID) column, the analyte zone is directed into a microfluidic chip containing a nanospray emitter and an electrospray ionization probe. By integrating high speed LC separation, multiplexed mass spectrometry, and microchip electrospray, high sensitivity is achieved. We have observed peak widths of approximately 30 s, with an equivalent time for a typical, postcolumn, infusion (about 2 s) used in nanospray LC. This allows multiple protein samples to be analyzed in the time between runs. A variety of proteins ranging from small peptides (6-12 kDa) to intact proteins (molecular weight, 26 kDa ac619d1d87
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